JP2007232985A - トナーの製造方法 - Google Patents
トナーの製造方法 Download PDFInfo
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- JP2007232985A JP2007232985A JP2006053744A JP2006053744A JP2007232985A JP 2007232985 A JP2007232985 A JP 2007232985A JP 2006053744 A JP2006053744 A JP 2006053744A JP 2006053744 A JP2006053744 A JP 2006053744A JP 2007232985 A JP2007232985 A JP 2007232985A
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- toner
- binder resin
- acid
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- pressure vessel
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Abstract
【解決手段】 トナー原料の混練物を分散剤の水分散液と混合して造粒を行うに際し、造粒系内を加熱加圧するとともに、造粒機として、円筒状耐圧性容器2と、回転ローター3と、追従スクリーン4,5と、固定スクリーン6とを含む高速回転分散型造粒機1を用い、トナー原料の混練物に剪断力とともに衝突力を付与する。
【選択図】 図1
Description
結着樹脂と着色剤とを含むトナー原料の混練物への剪断力および衝突力の付与が、
内部空間を有して密閉可能な円筒状耐圧容器と、
円筒状耐圧容器の内部空間において該耐圧容器の厚み方向におけるいずれか一方の面または両方の面に支持され、該耐圧容器と同一の軸心を有して回転駆動可能に設けられる回転ローターと、
回転ローターの周囲に円筒状耐圧容器と同一の軸心を有し、回転ローターの回転に追従回転可能に設けられ、周壁に複数の液体流過用スリットが形成された筒状または桶状の追従スクリーンと、
追従スクリーンの周囲に円筒状耐圧容器と同一の軸心を有するように設けられ、周壁に複数の液体流過用スリットが形成された筒状または桶状の固定スクリーンとを含む造粒機を用いて行われることを特徴とする。
本工程では、トナー原料の混練物を調製する。トナー原料としては結着樹脂および着色剤を使用し、さらに離型剤、電荷制御剤などの一般的なトナー用添加剤を使用してもよい。
本工程では、分散剤の水溶液または水分散液を調製する。以後、特に断らない限り、水溶液と水分散液とをまとめて水分散液と総称する。分散剤の水分散液は、たとえば、分散剤を水に溶解または分散させることによって調製される。
本工程では、トナー原料の混練物と分散剤の水分散液とを混合する。この混合は、分散剤の水分散液にトナー原料の混練物を添加して行うのが好ましい。トナー原料の混練物と分散剤の水分散液との混合割合は特に制限されず、結着樹脂の種類、離型剤の種類、分散剤の種類、分散剤の水分散液における分散剤濃度などの各種条件に応じて広い範囲から適宜選択できるけれども、トナー原料の混練物100重量部に対して分散剤を0.1〜10重量部使用するのが好ましく、0.1〜3.0重量部使用するのがさらに好ましい。
本工程では、トナー原料の混練物と分散剤の水分散液との混合物に、加熱加圧下に剪断力と衝突力とを付与し、該混練物の微細粒子を得る造粒を行う。なお、トナー原料の混練物と分散剤の水分散液との混合および造粒を同時に行っても良い。
本工程では、造粒工程で得られる微細粒子を含む水分散液を室温程度まで冷却し、該水分散液中の微細粒子の冷却固化物を遠心分離、濾過などの一般的な固液分離手段によって分取し、乾燥させることによって本発明のトナーを得る。本発明のトナーは、たとえば、粒径5μm程度の粒径が非常に小さいトナーであり、粒度分布の幅が従来のトナーよりも狭く、かつ形状も均一である。
[混練物調製工程]
カーボンブラック粒子(着色剤、商品名:NIPX60、デグザ社製)8部、エステルワックス粒子(離型剤、商品名:WEP−5、日本油脂(株)製、融点82℃)5部、ポリエステル(結着樹脂、軟化温度(Tm)125℃、ガラス転移温度(Tg)58℃、花王(株)製)90部および帯電制御剤(商品名:TRH、保土谷化学工業(株)製)2部を、混合機(商品名:ヘンシェルミキサー、三井鉱山(株)製)にて混合し、原料混合物を得た。得られた原料混合物を、2軸押出混練機(商品名:PCM30、(株)池貝製)にて、混練温度T1を結着樹脂の軟化温度(Tm)よりも15℃高い温度(Tm+15℃)である140℃として混練し、混練物を得た。2軸押出混練機のスクリュには、外径寸法Dが30mmであり、回転軸線方向の長さ寸法Lが1mであり、外径寸法Dに対する長さ寸法Lの比(L/D)が33であるスクリュを用いた。
イオン交換水(導電率8μS/cm)に、スチレン−アクリル酸共重合体アンモニウム塩(分散剤、商品名:ジョンクリル52、ジョンソンポリマー(株)製)を固形分濃度が20重量%(固形分濃度)になるように混合して溶解させ、分散剤の20%水溶液を調製した。
上記で得られた混練物100部および分散剤の20%水溶液400部を、圧力調整弁、加熱手段およびローターステータ式撹拌手段を備える金属製の円筒状耐圧性容器(高速回転分散型造粒機、商品名:泡レスミキサー、日本ビーイーイー(株)製)に投入し、回転ローター(外径30mm)の回転速度:10000rpm/分、造粒温度:150℃、造粒圧力:0.17MPaの条件で10分間造粒を行い、トナー原料の混練物の微細粒子を調製した。
円筒状耐圧性容器内にて、回転ローターの回転速度10000rpm/分を維持しながら加熱を停止し、微細粒子を含む分散剤の水分散液の液温が20℃になるまで冷却を行った。冷却後、微細粒子を含む分散剤の水分散液を円筒状耐圧性容器から取り出し、濾過を行って微細粒子を分取し、真空乾燥機にて温度50℃で8時間乾燥させ、本発明のトナーを得た。得られたトナー粒子について、下記の粒度測定法によって体積平均粒径および変動係数(CV値)を求めたところ、体積平均粒径は5.3μm、CV値は32であった。得られたトナー粒子100部に、疎水化処理したコロイダルシリカ(商品名:RX−300、日本アエロジル(株)製)0.6部を添加し、ヘンシェルミキサーを用いて混合し、本発明のトナーを得た。
塩化ナトリウム(1級)の1重量%水溶液(電解液)20mlに、アルキルベンゼンスルホン酸塩(分散剤)0.5mlおよびトナー試料3mgを順次添加し、5分間超音波分散した後、全量が100mlになるように塩化ナトリウム(1級)の1重量%水溶液を添加し、再度5分間超音波分散して測定用試料とした。この測定用試料について、コールターカウンターTA−III(商品名、コールター社製)を用い、アパーチャ径:100μm、測定対象粒径:個数基準で2〜40μm、測定粒子数:50000カウントの条件下に測定を行い、体積平均粒子径および体積粒度分布における標準偏差を求めた。変動係数(CV値)については、下記式に基づいて算出した。
CV値(%)=〔体積粒度分布における標準偏差〕/〔体積平均粒子径〕×100
スチレン80.5部、n−ブチルアクリレート19.5部、ポリメタクリル酸エステルマクロモノマー0.3部、ジビニルベンゼン0.5部、t−ドデシルメルカプタン1.2部、カーボンブラック(商品名:#25、三菱化学(株)製)7部、帯電制御剤(商品名:スピロンブラックTRH、保土ヶ谷化学工業(株)製)1部および離型剤(フィッシャートロプシュワックス、商品名:パラプリント スプレイ 30、サゾール社製)2部を超音波乳化機にて微分散化処理して液滴が安定するまで攪拌し、そこにt−ブチルパーオキシ−2−エチルヘキサノエート(重合開始剤、商品名:パーブチルO、日本油脂(株)製)6部を添加した後、造粒機(商品名:エバラマイルダー、(株)荏原製作所製)を用いて高剪断攪拌して、単量体混合物の液滴を造粒した。得られた単量体混合物の液滴の水分散液を、攪拌翼を装着した反応器に入れて85℃で重合反応を開始させ、重合転化率がほぼ100%に達した後、水溶性開始剤(2,2’−アゾビス(2−メチル−N−(2−ハイドロキシエチル)−プロピオンアミド、商品名:VA−086、和光純薬工業(株)製)0.3部を反応器に入れて4時間重合を継続した後、冷却して反応を停止し、着色重合体粒子の水分散液を得た。このとき、着色重合体粒子の水分散液の固形分濃度は27重量%であった。この着色重合体粒子の分散液にpH4になるまで硫酸を添加し、着色重合体粒子表面の水酸化マグネシウムを水に可溶化させた。この水酸化マグネシウムを可溶化させた分散液を連続式ベルトフィルター(商品名:イーグルフィルター、住友重機械工業(株)製)に供給し、固形分に対し10倍量のイオン交換水で洗浄・脱液した。ここで得られた湿潤した着色重合体粒子ケーキの含水率は35%であった。
透過型電子顕微鏡(Transmission Electron Microscope、略称TEM)を用いて実施例1および比較例1のトナーを観察し、トナーのTEM画像を画像解析ソフト(商品名:A像くん、旭化成エンジニアリング(株)製)を用いて解析し、観察領域内に含まれるすべての顔料の面積を合計した面積の観察領域の全面積に対する比率(以後、「全顔料の面積率」と称する)Dtotalおよび観察領域内に含まれる粒径0.1μm以下の顔料の面積を合計した面積の観察領域の全面積に対する比率(以後、「粒径0.1μm以下の顔料の面積率」と称する)D0.1を求めた。得られた全顔料の面積率Dtotalおよび粒径0.1μm以下の顔料の面積率D0.1から、下記式(1)に基づいて分散率D(%)を算出した。算出された分散率D(%)を顔料の分散性の評価指標として用い、次の基準に基づいて顔料の分散性を評価した。○:優れている。分散率Dが90%以上である。△:実用可能である。分散率Dが85%以上90%未満である。×:実用が困難である。分散率Dが85%未満である。
D(%)=D0.1/Dtotal×100 …(1)
実施例1または比較例1のトナーを、定着装置を取外した市販画像形成装置(商品名:デジタルフルカラー複合機AR−150、シャープ(株)製)の現像装置の現像槽に充填し、記録用紙(商品名:フルカラー専用紙PP106A4C、シャープ(株)製)にトナー付着量が0.6mg/cm2になるように調整して、べた画像部を含むテスト画像を未定着の状態で形成した。形成された未定着画像を、外部定着機によって記録用紙に定着させ、得られた定着画像を評価用画像とした。外部定着機には、市販の画像形成装置(商品名:デジタルフルカラー複合機AR−150、シャープ株式会社製)を改造した定着装置を用いた。得られた評価用画像について、分光測色濃度計(商品名:X−Rite938、日本平版印刷機材(株)製)を用いて、べた画像部の光学濃度を測定した。測定された光学濃度を画像濃度の評価指標として用い、以下の基準に基づいて画像濃度を評価した。
○:優れている。光学濃度が1.35以上である。
△:実用可能である。光学濃度が1.30以上1.35未満である。
×:実用が困難である。光学濃度が1.30未満である。
まず白色度計(商品名:Z−Σ90 COLOR MEASURING SYSTEM、日本電色工業(株)製)を用い、JIS P0138に規定されるA4判の記録用紙(フルカラー専用紙PP106A4C)について、JIS P8148に規定される白色度を測定し、この値を第1測定値W1とした。実施例1または比較例1のトナーを市販複写機(商品名:AR−620、シャープ(株)製)の現像装置の現像槽に投入し、JIS P8148に規定の白色度を測定した記録用紙3枚に、直径55mmの白円部とそれを取囲む黒べた部とを含むサンプル画像を形成し、得られた画像を評価用画像とした。前述の白色度計を用い、各評価用画像の白円部の白色度を測定し、これらの平均値を算出し、この平均値を第2測定値W2とした。第1測定値W1および第2測定値W2から下記式(2)に基づいてかぶり濃度W(%)を算出した。算出されたかぶり濃度Wをかぶり度合の評価指標として用い、以下の基準に基づいてかぶり度合を評価した。○:優れている。かぶり濃度Wが1.0%未満である。△:実用可能である。かぶり濃度Wが1.0%以上1.5%未満である。×:実用が困難である。かぶり濃度Wが1.5%以上である。
W(%)={(W1−W2)/W1}×100 …(2)
実施例1または比較例1のトナーを市販の複写機(AR−620)の現像装置の現像槽に投入し、記録用紙(フルカラー専用紙PP106A4C)にべた画像部を含む所定のチャートを複写し、べた画像部において記録用紙の単位面積あたりに転写されたトナーの重量(以後「転写トナー量」と称す)Mp(mg/cm2)を測定した。また複写に用いた感光体のべた画像部が形成されていた部分の単位面積あたりの残留トナー重量(以後「残留トナー量」と称す)Md(mg/cm2)を測定した。トナーの重量は、温度20℃、相対湿度50%RHの環境下にて測定した。測定した転写トナー量Mpおよび残留トナー量Mdから、下記式(3)に基づいて転写率T(%)を算出した。算出された転写率Tを転写性の評価指標として用い、以下の基準に基づいて転写性を評価した。○:優れている。転写率Tが90%以上である。×:実用が困難である。転写率Tが90%未満である。
T(%)={Mp/(Md+Mp)}×100 …(3)
2 円筒状耐圧容器
2a 内部空間
2b 外壁
3 回転ローター
3a 回転軸
3b 攪拌羽根
4,5 追従スクリーン
6 固定スクリーン
7 液体流過用スリット
8 矢符
Claims (9)
- 加熱加圧下および分散剤の存在下、水中にて、結着樹脂と着色剤とを含むトナー原料の混練物に剪断力と衝突力とを付与して造粒を行うことを特徴とするトナーの製造方法。
- 結着樹脂がポリエステル、アクリル樹脂、ポリウレタンおよびエポキシ樹脂から選ばれる1種または2種以上であることを特徴とする請求項1記載のトナーの製造方法。
- 結着樹脂がポリエステルであ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。
- トナー原料の混練物が、結着樹脂および着色剤とともに、離型剤および/または電荷制御剤を含む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。
- 分散剤が水溶性高分子分散剤であ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。
- 水溶性高分子分散剤が、ポリオキシアルキレンアルキルアリールエーテル硫酸塩およびポリオキシアルキレンアルキルエーテル硫酸塩から選ばれる1種または2種以上の水溶性高分子分散剤であることを特徴とする請求項5記載のトナーの製造方法。
- 50〜150℃の加熱下および0.13〜0.3MPaの加圧下に、トナー原料の混練物に剪断力と衝突力とが付与されることを特徴とする請求項1〜6のいずれか1つに記載のトナーの製造方法。
- 結着樹脂と着色剤とを含むトナー原料の混練物への剪断力および衝突力の付与が、
内部空間を有して密閉可能な円筒状耐圧容器と、
円筒状耐圧容器の内部空間において該耐圧容器の厚み方向におけるいずれか一方の面または両方の面に支持され、該耐圧容器と同一の軸心を有して回転駆動可能に設けられる回転ローターと、
回転ローターの周囲に円筒状耐圧容器と同一の軸心を有し、回転ローターの回転に追従回転可能に設けられ、周壁に複数の液体流過用スリットが形成された筒状または桶状の追従スクリーンと、
追従スクリーンの周囲に円筒状耐圧容器と同一の軸心を有するように設けられ、周壁に複数の液体流過用スリットが形成された筒状または桶状の固定スクリーンとを含む造粒機を用いて行われることを特徴とする請求項1〜7のいずれか1つに記載のトナーの製造方法。 - 結着樹脂と着色剤とを含むトナー原料の混練物が、トナー原料をオープンロール式混練機にて混練することによって得られるものであることを特徴とする請求項1〜8のいずれか1つに記載のトナーの製造方法。
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US7851120B2 (en) * | 2007-12-13 | 2010-12-14 | Kabushiki Kaisha Toshiba | Developing agent and method for producing the same |
US8652745B2 (en) | 2008-01-16 | 2014-02-18 | Penn Color, Inc. | Ink toner particles with controlled surface morphology |
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