JP4445983B2 - トナーの製造方法 - Google Patents
トナーの製造方法 Download PDFInfo
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- JP4445983B2 JP4445983B2 JP2007178960A JP2007178960A JP4445983B2 JP 4445983 B2 JP4445983 B2 JP 4445983B2 JP 2007178960 A JP2007178960 A JP 2007178960A JP 2007178960 A JP2007178960 A JP 2007178960A JP 4445983 B2 JP4445983 B2 JP 4445983B2
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Description
予備粉砕工程で得られる粗粉スラリーを加熱加圧下で耐圧ノズルに通過させてトナー粗粉をさらに粉砕し、トナー粗粉よりも体積平均粒子径の小さいトナー微粉を含みかつ加熱加圧状態にある微粉スラリーを得る微粉砕工程と、
微粉砕工程で得られる微粉スラリーを、加圧加熱下でコイル状配管に流過させることで、微粉スラリー中に渦流を発生させてトナー微粉を凝集させるとともに、得られるトナー微粉の凝集物を粉砕して凝集物の粒度を調整する凝集粉砕工程と、
凝集粉砕工程で得られる微粉スラリーを冷却する冷却工程と、
冷却工程で冷却される微粉スラリーを減圧する減圧工程とを含み、
微粉砕工程では、前記耐圧ノズルとして、複数の液体流過路が長手方向に平行に形成された耐圧性の多重ノズルを用い、
予備粉砕工程では、回転自在に設けられる円筒状ステータ部材と、円筒状ステータ部材の内部において回転自在に設けられる円柱状ロータ部材とを含み、円筒状ステータ部材と円柱状ロータ部材との間隙が50μm以下であるコロイドミルを用い、トナー原料の溶融混練物と液体との混合物をコロイドミルにおける円筒状ステータ部材と円柱状ロータ部材との間隙に通過させることによってトナー粗粉の、下記式で表わされる変動係数が25〜45%になるようにトナー原料の溶融混練物を粉砕することを特徴とするトナーの製造方法である。
変動係数(%)=(体積粒度分布における標準偏差/体積平均粒子径)×100
さらに本発明のトナーの製造方法は、予備粉砕工程と微粉砕工程との間に、予備粉砕工程で得られる粗粉スラリーに分散剤を添加する粗粉スラリー安定化工程を設けることを特徴とする。
また微粉砕工程では、前記耐圧ノズルとして、複数の液体流過路が長手方向に平行に形成された耐圧性の多重ノズルを用い、予備粉砕工程では、回転自在に設けられる円筒状ステータ部材と、円筒状ステータ部材の内部において回転自在に設けられる円柱状ロータ部材とを含み、円筒状ステータ部材と円柱状ロータ部材との間隙が50μm以下であるコロイドミルを用い、トナー原料の溶融混練物と液体との混合物をコロイドミルにおける円筒状ステータ部材と円柱状ロータ部材との間隙に通過させることによってトナー粗粉の、変動係数が25〜45%になるようにトナー原料の溶融混練物を粉砕する。
また、予備粉砕工程において、トナー粗粉の変動係数が25〜45%になるようにトナー原料の溶融混練物を均一粉砕することによって、微粒化工程に要する時間を短縮化し、かつ電力、燃料などのエネルギー減の使用量を一層低減化できる。
また、予備粉砕工程において、溶融混練物を粉砕する粉砕装置として、回転自在に設けられる円筒状ステータ部材と円筒状ステータ部材の内部において回転自在に設けられる円柱状ロータ部材とを含むコロイドミルを用いるのが好ましい。すなわち、トナー原料の溶融混練物と液体との混合物をコロイドミルにおける円筒状ステータ部材と円柱状ロータ部材との間隙に通過させることによって、トナー粗粉を効率良くかつ比較的短時間で得ることができ、トナー粗粉表面に付着する気泡数がより一層減少する。また、トナー粗粉の形状が揃い、粒度分布が狭くなる。
さらに、円筒状ステータ部材と円柱状ロータ部材との間隙を50μm以下、好ましくは40〜50μm(40μm以上、50μm以下)にすることによって、適度に小径化されたトナー粗粉が得られる。これは、微粉砕工程における耐圧ノズルの目詰まり防止などに有効である。
トナー原料の溶融混練物は、たとえば、各種トナー原料を混合機で乾式混合した後、結着樹脂の溶融温度以上の温度(通常は80〜200℃程度、好ましくは100〜150℃程度)に加熱しながら、溶融混練することにより製造できる。ここで混合機としては公知のものを使用でき、たとえば、ヘンシェルミキサ(商品名、三井鉱山(株)製)、スーパーミキサー(商品名、(株)カワタ製)、メカノミル(商品名、岡田精工(株)製)などのヘンシェルタイプの混合装置、オングミル(商品名、ホソカワミクロン(株)製)、ハイブリダイゼーションシステム(商品名、(株)奈良機械製作所製)、コスモシステム(商品名、川崎重工業(株)製)などが挙げられる。溶融混練には、二軸押し出し機、三本ロール、ラボブラストミルなどの一般的な混練機を使用できる。さらに具体的には、たとえば、TEM−100B(商品名、東芝機械(株)製)、PCM−65/87(商品名、(株)池貝製)などの1軸もしくは2軸の押出機、ニーディックス(商品名、三井鉱山(株)製)などのオープンロール方式のものが挙げられる。
予備粉砕工程S1では、液体中にてトナー原料の溶融混練物(以下特に断わらない限り単に「溶融混練物」とする)を粉砕して、トナー粗粉を含む粗粉スラリーを調製する。予備粉砕工程S1では、具体的には、液体と溶融混練物との混合物に対して、湿式粉砕が可能な粉砕装置によって粉砕処理を施すことにより行われる。ここで、液体としては、トナー粗粉を溶解せずかつ均一に分散させ得る液体であれば特に制限されないけれども、工程管理の容易さ、全工程終了後の廃液処理などを考慮すると、水が好ましい。また、液体と溶融混練物との使用割合は特に制限されず、使用する粉砕装置に応じて、粉砕処理が円滑に進行する使用割合を適宜選択すればよい。粉砕装置としては、湿式粉砕が可能なものであれば特に制限されず、たとえば、振動ミル、自動乳鉢、サンドミル、ダイノーミル、コボールミル、アトライター、遊星ボールミル、ボールミル、コロイドミルなどが挙げられる。これらの中でも、コロイドミルが好ましい。
微粉砕工程S2では、予備粉砕工程S1で得られる粗粉スラリーを加熱加圧下で耐圧ノズルに通過させてトナー粗粉をさらに粉砕し、トナー粗粉よりも体積平均粒子径の小さいトナー微粉を含みかつ加熱加圧状態にある微粉スラリーを調製する。なお、粗粉スラリーは耐圧ノズルを1度も通過していないスラリーであり、微粉スラリーは耐圧ノズルを少なくとも1度通過したスラリーである。
CV値(%)=(体積粒度分布における標準偏差/体積平均粒子径)×100
冷却工程S3では、微粉砕工程S2で得られる加熱加圧状態にある微粉スラリーを冷却する。具体的には、たとえば、微粉砕工程S2において耐圧ノズルから排出される微粉スラリーを液体冷却機に導入することによって冷却する。冷却温度には制限はないけれども、1つの目安を挙げれば、たとえば、液温30℃以下まで冷却すると、該スラリーに付加される圧力は5〜80MPa程度に減圧される。
減圧工程S4では、冷却工程S3で得られる微粉スラリーに付加される圧力を、バブリング(泡の発生)が起こらない程度の圧力まで減圧する。冷却工程S3から減圧工程S4に供給される微粉スラリーは、5〜80MPa程度に加圧された状態にある。減圧工程では、徐々に段階的に減圧されるように操作するのが好ましい。この減圧操作には、国際公開第03/059497号パンフレットに記載の多段減圧装置を用いるのが好ましい。
撹拌容器21に微粉スラリー22が収容された状態で、撹拌手段23のインペラ26が回転すると、スラリー流入孔30の上方に存在する微粉スラリー22がスラリー流入孔30を介して矢符36方向に流れてプレート間空間部33に流入する。また第1スクリーン部材28aよりも内側の微粉スラリー22は、インペラ26の回転によって、インペラ26の回転軸31を中心とし、インペラ26の回転軸に垂直な平面内に存在する仮想円の半径方向外方に吐出される。吐出された微粉スラリー22は、第1スクリーン部材28akスリット35、第2スクリーン部材28aのスリット35および第3スクリーン部材28cのスリット35を順に流過し、プレート間空間部33から流出する。プレート間空間部33から流出する微粉スラリー22は、インペラ26の回転軸に垂直な平面内に存在する仮想円の円周方向の流れ成分を含まない。したがって、微粉スラリー22は半径方向外方に放射状に撹拌手段23から流出し、撹拌容器21の内壁面に衝突するとき、微粉スラリー22には渦流が発生しない。
[予備粉砕工程]
ポリエステル(重量平均分子量:80000、Mw/Mn=24)88.5部、帯電制御剤(商品名:N4P、クラリアントジャパン(株)製)2部、カルナバワックス7.5部および着色剤(FC1469)10部を混合機(商品名:ヘンシェルミキサー、三井鉱山(株)製)で混合し、得られたトナー原料混合物を二軸押出機(商品名:PCM−30、(株)池貝製)にてシリンダ温度145℃、バレル回転数300rpmで溶融混練し、トナー原料の溶融混練物を調製した。この溶融混練物10部およびイオン交換水100部をコロイドミル(商品名:PUCコロイド・ミル60型、日本ボールバルブ(株)製、間隙d1:40μm)によって粉砕して粗粉スラリーを調製した。なお、粗粉スラリー中に含まれるトナー粗粉の体積平均粒子径が100μm未満になるまで、粉砕を繰り返し行い、体積平均粒子径が65μm、変動係数(CV値)37、最小粒径7.7μm、最大粒径300.5μmのトナー粗粉を含む粗粉スラリーを調製した。
粗粉スラリー94部に高分子系分散剤(商品名:ジョングリル70、ジョンソンポリマー社製)6部を添加して混合した。
粗粉スラリー安定化工程で得られた粗粉スラリーを耐圧性密閉容器中で210MPaおよび70℃に加圧加熱し、耐圧性密閉容器に取り付けられた耐圧性配管から該耐圧性配管の出口に取り付けられた耐圧ノズルに供給してトナー粗粉の微粉砕を行い、体積平均粒径0.97、変動係数31のトナー微粉を含む微粉スラリーを調製した。耐圧ノズルはダイヤモンド製で、孔径0.085mmの液体流過孔2本がノズルの長手方向において1.0mmの間隔をあけてほぼ平行になるように形成された長さ0.5cmの耐圧性多重ノズルである。
耐圧ノズルから排出される微粉スラリーを、耐圧ノズルの出口に接続される蛇管式冷却機に導入し、冷却を行った。蛇管式冷却機出口での微粉スラリーの温度は30℃、微粉スラリーに付加される圧力は35MPaであった。
蛇管式冷却機出口から排出される微粉スラリーを、冷却機出口に接続されるコイル状配管内に導入し、トナー微粉の凝集および生成する凝集粒子の粉砕を行い、体積平均粒子径5.3μm、変動係数19の凝集粒子を調製した。コイル状配管は、コイル内径4.0mm、コイル曲率半径38mm、コイル巻き数54であった。
コイル状配管出口から排出される微粉スラリー(凝集粒子含有スラリー)を、コイル状配管出口に接続される多段減圧装置に導入し、減圧を行った。多段減圧装置は、内径の異なる5個のステンレス鋼製パイプ状部材をシール部材(Oリング)にて連結してなるものである。パイプ状部材の内径は、多段減圧装置の入口から順番に1mm、0.9mm、0.75mm、0.5mm、0.2mmであった。
多段減圧装置から排出されるスラリーから凝集粒子(トナー)を濾取し、純水によって洗浄した後、熱風乾燥し、本発明トナーを製造した。
微粉砕工程において、微粉スラリーを耐圧ノズルに通過させる回数を10回(実施例2)または2回(実施例3)に変更する以外は、実施例1と同様にして、本発明のトナー(凝集粒子)を製造した。トナー粗粉、トナー微粉およびトナーの体積平均粒子径(μm)および変動係数を表1に示す。
コロイドミル(PUCコロイド・ミル60型)における間隙d1を40μmから50μmに変更する以外は、実施例1と同様にして、本発明のトナー(凝集粒子)を製造した。トナー粗粉、トナー微粉およびトナーの体積平均粒子径(μm)および変動係数を表1に示す。
冷却工程の後に減圧工程を行い、かつ減圧工程の後に下記の凝集工程を行う以外は、実施例1と同様にして、本発明のトナー(凝集粒子)を製造した。トナー粗粉、トナー微粉およびトナーの体積平均粒子径(μm)および変動係数を表1に示す。
多段減圧装置から排出される微粉スラリー100部と、塩化ステアリルトリメチルアンモニウム(商品名:コータミン86W、花王(株)製)の20%水溶液5部とを、造粒装置(商品名:ニュージェネレーションミキサNGM−1.5TL、(株)美粒製)に投入し、75℃、2000rpmで30分間撹拌した後、85℃に昇温し、さらに2時間撹拌した。未凝集のトナー微粉を凝集させるために、昇温後に水300gを追加し、室温まで急冷し、微粉スラリー(凝集粒子含有スラリー)を調製した。なお、ここで使用される造粒装置は、図5に示す造粒装置100と同じ構造を有するものである。この造粒装置において、撹拌手段23は、撹拌容器21内の微粉スラリー液面と、第1カバープレート24を臨む側の撹拌翼上端との距離Hが2.0cm、撹拌容器21の底面と第2カバープレート25の第1カバープレート24を臨む側とは反対側の面との距離d2が0.5cmになる位置に配置される。撹拌容器21の内径Dは10.5cm、撹拌翼先端速度は3.14m/s、波の高さは10mmであった。
微粉砕工程において、微粉スラリーを耐圧ノズルに通過させる回数を15回(比較例1)または1回(比較例2)に変更する以外は、実施例1と同様にして、比較用のトナー(凝集粒子)を製造した。トナー粗粉、トナー微粉およびトナーの体積平均粒子径(μm)および変動係数を表1に示す。
コロイドミル(PUCコロイド・ミル60型)における間隙d1を40μmから60μmに変更する以外は、実施例1と同様にして操作を行ったところ、微粉砕工程において耐圧ノズル中にてトナー粗粉による目詰まりが発生し、その後の工程を実施できなかった。粗粉スラリーの体積平均粒子径(μm)および変動係数を表1に示す。
実施例1と同様にして、トナー原料の溶融混練物を調製した。この溶融混練物を室温まで冷却した後、カッターミル(商品名:VM−16、オリエント(株)製)で粉砕し、粒径500〜800μmのトナー粗粉を調製した。このトナー粗粉10部と、高分子系分散剤(ジョングリル70)の30%水溶液1.7部と、イオン交換水90部を混合し、粗粉スラリーを調製した。この粗粉スラリーを168MPaの加圧下に内径0.3mmの流過孔を有するノズル長0.5cmのノズルに通過させて予備粉砕を行い、該スラリー中のトナー粗粉の体積平均粒子径が100μm未満(92μm)になるように調整した。
コロイドミルをPUCコロイド・ミル60型からディスパミルD(商品名、ホソカワミクロン(株)製)に変更し、かつ間隙d1を40μmから200μmに変更する以外は、実施例1と同様にして操作を行ったところ、微粉砕工程において耐圧ノズル中にてトナー粗粉による目詰まりが発生し、その後の工程を実施できなかった。粗粉スラリーの体積平均粒子径(μm)および変動係数を表1に示す。
2 ステータ部材
3 ロータ部材
4,8,12 矢符
5 耐圧ノズル
6 液体流過路
7 衝突壁
10 減圧ノズル
11 流路
21 撹拌容器
22 微粉スラリー
23 撹拌手段
24 第1カバープレート
25 第2カバープレート
26 インペラ
27 スクリーン部材
30 スラリー流入孔
31 回転軸
33 プレート間空間部
34 撹拌翼
35 スリット
100 画像形成装置
114 現像手段
Claims (6)
- 液体中にてトナー原料の溶融混練物を粉砕してトナー粗粉を含む粗粉スラリーを得る予備粉砕工程と、
予備粉砕工程で得られる粗粉スラリーを加熱加圧下で耐圧ノズルに通過させてトナー粗粉をさらに粉砕し、トナー粗粉よりも体積平均粒子径の小さいトナー微粉を含みかつ加熱加圧状態にある微粉スラリーを得る微粉砕工程と、
微粉砕工程で得られる微粉スラリーを、加圧加熱下でコイル状配管に流過させることで、微粉スラリー中に渦流を発生させてトナー微粉を凝集させるとともに、得られるトナー微粉の凝集物を粉砕して凝集物の粒度を調整する凝集粉砕工程と、
凝集粉砕工程で得られる微粉スラリーを冷却する冷却工程と、
冷却工程で冷却される微粉スラリーを減圧する減圧工程とを含み、
微粉砕工程では、前記耐圧ノズルとして、複数の液体流過路が長手方向に平行に形成された耐圧性の多重ノズルを用い、
予備粉砕工程では、回転自在に設けられる円筒状ステータ部材と、円筒状ステータ部材の内部において回転自在に設けられる円柱状ロータ部材とを含み、円筒状ステータ部材と円柱状ロータ部材との間隙が50μm以下であるコロイドミルを用い、トナー原料の溶融混練物と液体との混合物をコロイドミルにおける円筒状ステータ部材と円柱状ロータ部材との間隙に通過させることによってトナー粗粉の、下記式で表わされる変動係数が25〜45%になるようにトナー原料の溶融混練物を粉砕することを特徴とするトナーの製造方法。
変動係数(%)=(体積粒度分布における標準偏差/体積平均粒子径)×100 - 予備粉砕工程において、分散剤の非存在下にトナー原料の溶融混練物を粉砕することを特徴とする請求項1記載のトナーの製造方法。
- 予備粉砕工程において、粒径500μmを超えるトナー粗粉粒子を含まない粗粉スラリーを得ることを特徴とする請求項1または2記載のトナーの製造方法。
- 液体が水であることを特徴とする請求項1〜3のいずれか1つに記載のトナーの製造方法。
- 予備粉砕工程と微粉砕工程との間に、予備粉砕工程で得られる粗粉スラリーに分散剤を添加する粗粉スラリー安定化工程を設けることを特徴とする請求項1〜4のいずれか1つに記載のトナーの製造方法。
- 微粉スラリーを収容する容器と、容器内に設けられて容器に収容される微粉スラリーを撹拌する撹拌部材と、撹拌部材を囲むように設けられて厚み方向に貫通する複数の微粉スラリー流過孔が形成される2以上のスクリーン部材とを含む造粒装置を用いて、減圧工程後の微粉スラリーに含まれるトナー微粉を凝集させる凝集工程をさらに含むことを特徴とする請求項1〜5のいずれか1つに記載のトナーの製造方法。
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US12/167,519 US8163458B2 (en) | 2007-07-06 | 2008-07-03 | Method of manufacturing toner, toner, two-component developer, developing device, and image forming apparatus |
CN2008101356126A CN101339373B (zh) | 2007-07-06 | 2008-07-07 | 调色剂及其制造方法、双组分显影剂、显影装置及图像形成装置 |
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US5424162A (en) | 1992-11-24 | 1995-06-13 | Minolta Camera Kabushiki Kaisha | Toner for electrophotography containing wax-particles dispersed in binder resin |
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