JP6080621B2 - トナープロセス - Google Patents
トナープロセス Download PDFInfo
- Publication number
- JP6080621B2 JP6080621B2 JP2013047525A JP2013047525A JP6080621B2 JP 6080621 B2 JP6080621 B2 JP 6080621B2 JP 2013047525 A JP2013047525 A JP 2013047525A JP 2013047525 A JP2013047525 A JP 2013047525A JP 6080621 B2 JP6080621 B2 JP 6080621B2
- Authority
- JP
- Japan
- Prior art keywords
- toner
- particles
- temperature
- resin
- toner particles
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 2
- 229920002959 polymer blend Polymers 0.000 description 2
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- 150000003839 salts Chemical class 0.000 description 2
- 238000010583 slow cooling Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- LONCJFPVKZBTLG-UHFFFAOYSA-N 2-methylbuta-1,3-diene prop-1-enylbenzene Chemical compound CC(=C)C=C.CC=CC1=CC=CC=C1 LONCJFPVKZBTLG-UHFFFAOYSA-N 0.000 description 1
- KLWOORLBKQYYQC-UHFFFAOYSA-N 2-methylbuta-1,3-diene propyl prop-2-enoate Chemical compound CC(=C)C=C.CCCOC(=O)C=C KLWOORLBKQYYQC-UHFFFAOYSA-N 0.000 description 1
- NRDDLSFHZLETFD-UHFFFAOYSA-N 2-methylbuta-1,3-diene;methyl 2-methylprop-2-enoate Chemical compound CC(=C)C=C.COC(=O)C(C)=C NRDDLSFHZLETFD-UHFFFAOYSA-N 0.000 description 1
- HNJKLOSHGNUTBM-UHFFFAOYSA-N 2-methylbuta-1,3-diene;methyl prop-2-enoate Chemical compound CC(=C)C=C.COC(=O)C=C HNJKLOSHGNUTBM-UHFFFAOYSA-N 0.000 description 1
- ROGIWVXWXZRRMZ-UHFFFAOYSA-N 2-methylbuta-1,3-diene;styrene Chemical compound CC(=C)C=C.C=CC1=CC=CC=C1 ROGIWVXWXZRRMZ-UHFFFAOYSA-N 0.000 description 1
- CKRJGDYKYQUNIM-UHFFFAOYSA-N 3-fluoro-2,2-dimethylpropanoic acid Chemical compound FCC(C)(C)C(O)=O CKRJGDYKYQUNIM-UHFFFAOYSA-N 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- ISCIUIIRLMFIQC-UHFFFAOYSA-N C=CC=C.C=CC#N.OC(=O)C=C.C=CC1=CC=CC=C1 Chemical compound C=CC=C.C=CC#N.OC(=O)C=C.C=CC1=CC=CC=C1 ISCIUIIRLMFIQC-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
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- 229910000288 alkali metal carbonate Inorganic materials 0.000 description 1
- 150000008041 alkali metal carbonates Chemical class 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
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- LKAVYBZHOYOUSX-UHFFFAOYSA-N buta-1,3-diene;2-methylprop-2-enoic acid;styrene Chemical compound C=CC=C.CC(=C)C(O)=O.C=CC1=CC=CC=C1 LKAVYBZHOYOUSX-UHFFFAOYSA-N 0.000 description 1
- WOYXYXOSUAZDIA-UHFFFAOYSA-N buta-1,3-diene;butyl 2-methylprop-2-enoate Chemical compound C=CC=C.CCCCOC(=O)C(C)=C WOYXYXOSUAZDIA-UHFFFAOYSA-N 0.000 description 1
- YIEXROAWVNRRMJ-UHFFFAOYSA-N buta-1,3-diene;butyl prop-2-enoate Chemical compound C=CC=C.CCCCOC(=O)C=C YIEXROAWVNRRMJ-UHFFFAOYSA-N 0.000 description 1
- UWWYTVDAXIVRAJ-UHFFFAOYSA-N buta-1,3-diene;ethyl 2-methylprop-2-enoate Chemical compound C=CC=C.CCOC(=O)C(C)=C UWWYTVDAXIVRAJ-UHFFFAOYSA-N 0.000 description 1
- UCPLVEOTDDIMJD-UHFFFAOYSA-N buta-1,3-diene;ethyl prop-2-enoate Chemical compound C=CC=C.CCOC(=O)C=C UCPLVEOTDDIMJD-UHFFFAOYSA-N 0.000 description 1
- KLIYQWXIWMRMGR-UHFFFAOYSA-N buta-1,3-diene;methyl 2-methylprop-2-enoate Chemical compound C=CC=C.COC(=O)C(C)=C KLIYQWXIWMRMGR-UHFFFAOYSA-N 0.000 description 1
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- UPMATSCYHGMGSE-UHFFFAOYSA-N butyl prop-2-enoate;prop-2-enenitrile;prop-2-enoic acid;styrene Chemical compound C=CC#N.OC(=O)C=C.C=CC1=CC=CC=C1.CCCCOC(=O)C=C UPMATSCYHGMGSE-UHFFFAOYSA-N 0.000 description 1
- WWPXOMXUMORZKI-UHFFFAOYSA-N butyl prop-2-enoate;prop-2-enenitrile;styrene Chemical compound C=CC#N.C=CC1=CC=CC=C1.CCCCOC(=O)C=C WWPXOMXUMORZKI-UHFFFAOYSA-N 0.000 description 1
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- REYZQLSIADJXGD-UHFFFAOYSA-N ethyl prop-2-enoate;2-methylbuta-1,3-diene Chemical compound CC(=C)C=C.CCOC(=O)C=C REYZQLSIADJXGD-UHFFFAOYSA-N 0.000 description 1
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- OIMDJNFWDDTLOZ-UHFFFAOYSA-N propyl prop-2-enoate;styrene Chemical compound CCCOC(=O)C=C.C=CC1=CC=CC=C1 OIMDJNFWDDTLOZ-UHFFFAOYSA-N 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
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- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 description 1
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- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
- G03G9/00—Developers
- G03G9/08—Developers with toner particles
- G03G9/093—Encapsulated toner particles
- G03G9/0935—Encapsulated toner particles specified by the core material
- G03G9/09357—Macromolecular compounds
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
- G03G9/00—Developers
- G03G9/08—Developers with toner particles
- G03G9/0802—Preparation methods
- G03G9/0804—Preparation methods whereby the components are brought together in a liquid dispersing medium
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
- G03G9/00—Developers
- G03G9/08—Developers with toner particles
- G03G9/0821—Developers with toner particles characterised by physical parameters
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
- G03G9/00—Developers
- G03G9/08—Developers with toner particles
- G03G9/087—Binders for toner particles
- G03G9/08784—Macromolecular material not specially provided for in a single one of groups G03G9/08702 - G03G9/08775
- G03G9/08795—Macromolecular material not specially provided for in a single one of groups G03G9/08702 - G03G9/08775 characterised by their chemical properties, e.g. acidity, molecular weight, sensitivity to reactants
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
- G03G9/00—Developers
- G03G9/08—Developers with toner particles
- G03G9/087—Binders for toner particles
- G03G9/08784—Macromolecular material not specially provided for in a single one of groups G03G9/08702 - G03G9/08775
- G03G9/08797—Macromolecular material not specially provided for in a single one of groups G03G9/08702 - G03G9/08775 characterised by their physical properties, e.g. viscosity, solubility, melting temperature, softening temperature, glass transition temperature
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
- G03G9/00—Developers
- G03G9/08—Developers with toner particles
- G03G9/093—Encapsulated toner particles
- G03G9/09307—Encapsulated toner particles specified by the shell material
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
- G03G9/00—Developers
- G03G9/08—Developers with toner particles
- G03G9/093—Encapsulated toner particles
- G03G9/09392—Preparation thereof
Description
2L反応器に、2種類のアモルファス樹脂(ポリエステルA(Mw=86,000、Tg開始=56℃、固形分35%)およびポリエステルB(Mw=19,400、Tg開始=60℃、固形分35%))の1:1混合物198g、結晶性ポリエステルC(Mw23,300、Mn=10,500、Tm=71℃、固形分35%)34g、2%界面活性剤(DOWFAX(登録商標)3A1、Dow Chemical Company)、ポリエチレンワックスエマルション(Tm=90℃、固形分30%、The International Group,Inc.(IGI))50g、黒色顔料(Nipex 35、Evonik Industries、Essen、DE)96kgおよびPigment PB 15:3分散物16gを、反応器の中で脱イオン水511gと混合した。0.3M硝酸を用い、トナースラリーのpHを4.2に調整した。その後、3000〜4000RPMで均質化しつつ、5分かけて硫酸アンモニウム溶液0.5pphを滴下した。反応器を500RPMに設定し、42℃に加熱してトナー粒子を凝集させた。目標粒径である4.8μmが達成されたら、この混合物に、DI水31g中のアモルファス樹脂167gのシェル混合物を加えた。次いで、反応物を46℃まで加熱した。トナー粒子の粒径5.3μmが得られたら、4% NaOH溶液を用いてスラリーのpHを4.5まで下げることによって融着を止めた。反応器の撹拌速度を200rpmまで下げ、次いで、pHが7.8に達するまでEDTAおよびさらなるNaOH溶液を加えた。反応器の温度を、表1に記載の望ましい融着温度まで上げた。望ましい温度になったら、pH5.7の酢酸ナトリウムバッファー溶液を用いてpHを7.0〜5.9に調整し、粒子を球形にした。約90分後、目標真円度に達したら(>0.965)、熱交換器を用いてスラリーを冷却した。遅い冷却は、温度を約0.75℃/分で下げつつ行った。急冷は、約1℃/分で温度を下げつつ行った。さまざまな融着条件を表1に詳細に記載している。
特注の器具でトナーペレットを作成することによって、誘電損失を決定した。バネ荷重による直径2インチの精密に磨いたプランジャを備えた型にトナーサンプルを入れ、約2000psiで2分間プレス処理した。プランジャ(1つの電極として作用する)と接触したままに維持しつつ、バネ荷重による支持体によってペレットを型に押し付け、ペレットに圧がかかった状態に維持し、これが対電極としても作用する。覆いをつけた1メートルのBNCケーブルを介してHP4263B LCR Meterを用い、周波数100KHzおよび1VACでキャパシタンス(Cp)および損失因子(D)を測定することによって誘電率および誘電損失を決定した。誘電定数は、以下のように計算した。E’=[Cp(pF)×厚み(mm)]/[8.854×Aeffective(m2)]。この値は8.854であり、真空誘電率エプシロン(ε)であるが、単位において、Cpがピコファラドであり、ファラドではない場合、厚みはmmであり、メートルではないことに注意されたい。Aeffectiveは、サンプルの有効面積である。誘電損失は、E*散逸率に等しく、サンプル中でどれだけ多くの電気の散逸が起こったか、つまり、コンデンサがどれだけ漏れているかである。値を単純化するために、これに1000を掛け算する。したがって、報告された誘電損失が70ということは、測定された誘電損失が70×10−3、つまり0.070であることを示す。
ベンチスケールのトナーのために使用したのと同じ成分を用い、同じ比率または相対量で試薬を用い、黒色ポリエステルEAトナーを調製した。合計60分間の再循環ループを用いつつ、CAVITRONホモジナイザによってスラリーを均質化し、最初の8分間に、2.96gの硫酸アルミニウムと36.5gのDI水とを混合してなる凝固剤をインラインで加えた。すべての凝固剤を加えたら、反応器のrpmを、100rpmから300rpmでの混合に設定して上げていく。次いで、スラリーをバッチ温度42℃で凝集させた。凝集中、コアと同じアモルファス樹脂で構成されるシェル配合物のpHを、硝酸を用いて3.3に調整し、これをバッチに加えた。バッチをさらに加熱し、目標粒径を得てもよい。目標粒径になったら、水酸化ナトリウム(NaOH)およびEDTAを用いてpHを7.8に調整し、凝集を凍結させた。反応器の温度(Tr)を所望の温度(表3を参照)まで上げつつ、このプロセスを続け、pH5.7の酢酸ナトリウム/酢酸バッファーを用いてpHを6.8〜6.0に調整すると、粒子が融着し始めた。2時間後、粒子は、真円度>0.965に達しており、熱交換器を用い、約1℃/分で急冷した。室温でトナーをDI水で3回洗浄し、ALJET THERMAJET乾燥器Model 4を用いて乾燥させた。
Claims (10)
- エマルション凝集トナー粒子を製造する方法であって、
第1のアモルファス樹脂と、結晶性樹脂と、ワックスと、導電性着色剤とを混合物になるように合わせることと、
前記混合物を凝集させて凝集粒子を作製することと、
前記結晶性樹脂の融点および前記ワックスの融点のいずれよりも低い温度で粒子を融着させることと、
前記トナー粒子を急冷して、70未満の誘電損失を有し、バルクナトリウムイオン濃度が1100ppm未満である、前記トナー粒子を得ることと、
を含む、方法。 - 前記トナー粒子が、前記結晶性樹脂および前記ワックスの融点より高い融着温度で、または0.8℃/分未満の温度低下速度で冷却するか、またはその両方で製造されたトナーと比較して誘電損失が低い、請求項1に記載の方法。
- 前記融着の温度が、80℃未満である、請求項1または2に記載の方法。
- 前記トナー粒子のバルクナトリウムイオン濃度が1000ppm未満である、請求項1〜3のいずれか一項に記載の方法。
- 前記凝集粒子の作製後、粒子の融着前に、樹脂エマルションを加えて、前記凝集粒子を覆うシェルを形成することを更に含む、請求項1〜4のいずれか一項に記載の方法。
- 前記シェルが、前記トナー粒子の重量の少なくとも25%の量で含まれる、請求項5に記載の方法。
- 前記トナー粒子の表面ナトリウムイオン濃度が、0.25atom%未満である、請求項1〜6のいずれか一項に記載の方法。
- 前記導電性着色剤が、黒色顔料を含む、請求項1〜7のいずれか一項に記載の方法。
- 前記トナー粒子が、乾燥重量に基づいて6重量%より多い前記導電性着色剤を含む、請求項1〜8のいずれか一項に記載の方法。
- 前記トナー粒子が、乾燥トナーの重量の25%から30%の量で存在するシェルを含む、請求項9に記載の方法。
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US9122179B2 (en) * | 2013-08-21 | 2015-09-01 | Xerox Corporation | Toner process comprising reduced coalescence temperature |
CN104330960A (zh) * | 2014-10-20 | 2015-02-04 | 中国科学院化学研究所 | 一种阴离子型纳米蜡乳液及其制备方法与应用 |
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