JP2008181041A - 磁性トナー及び画像形成方法 - Google Patents
磁性トナー及び画像形成方法 Download PDFInfo
- Publication number
- JP2008181041A JP2008181041A JP2007015975A JP2007015975A JP2008181041A JP 2008181041 A JP2008181041 A JP 2008181041A JP 2007015975 A JP2007015975 A JP 2007015975A JP 2007015975 A JP2007015975 A JP 2007015975A JP 2008181041 A JP2008181041 A JP 2008181041A
- Authority
- JP
- Japan
- Prior art keywords
- magnetic toner
- iron oxide
- magnetic
- magnetic iron
- acid
- 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.)
- Granted
Links
- 238000000034 method Methods 0.000 title claims abstract description 67
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- 229920005989 resin Polymers 0.000 claims abstract description 58
- 239000011347 resin Substances 0.000 claims abstract description 58
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 54
- 230000003647 oxidation Effects 0.000 claims abstract description 32
- 238000005259 measurement Methods 0.000 claims abstract description 28
- 230000000630 rising effect Effects 0.000 claims abstract description 20
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000001301 oxygen Substances 0.000 claims abstract description 14
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 14
- 230000008569 process Effects 0.000 claims abstract description 12
- 239000002245 particle Substances 0.000 claims description 44
- 238000012546 transfer Methods 0.000 claims description 41
- 239000011230 binding agent Substances 0.000 claims description 35
- 239000000463 material Substances 0.000 claims description 18
- 230000004913 activation Effects 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 6
- 238000007639 printing Methods 0.000 abstract description 20
- 235000013980 iron oxide Nutrition 0.000 description 94
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 49
- 239000007864 aqueous solution Substances 0.000 description 44
- -1 aliphatic alcohols Chemical class 0.000 description 36
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 33
- 239000000843 powder Substances 0.000 description 30
- 238000004519 manufacturing process Methods 0.000 description 24
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- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 14
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 14
- 239000000243 solution Substances 0.000 description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 13
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 13
- 229910052782 aluminium Inorganic materials 0.000 description 12
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- 150000002148 esters Chemical class 0.000 description 12
- 229930195733 hydrocarbon Natural products 0.000 description 12
- 150000002430 hydrocarbons Chemical class 0.000 description 12
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 12
- 239000011701 zinc Substances 0.000 description 12
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 11
- 229920001577 copolymer Polymers 0.000 description 11
- 239000003054 catalyst Substances 0.000 description 10
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- 125000004386 diacrylate group Chemical group 0.000 description 10
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- 238000009826 distribution Methods 0.000 description 9
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 9
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 9
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 8
- 150000008064 anhydrides Chemical class 0.000 description 8
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 238000010992 reflux Methods 0.000 description 8
- 239000004115 Sodium Silicate Substances 0.000 description 7
- 239000011247 coating layer Substances 0.000 description 7
- 239000013078 crystal Substances 0.000 description 7
- 235000014113 dietary fatty acids Nutrition 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 239000000194 fatty acid Substances 0.000 description 7
- 229930195729 fatty acid Natural products 0.000 description 7
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical class [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 description 7
- 229910052911 sodium silicate Inorganic materials 0.000 description 7
- 238000003756 stirring Methods 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 7
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 6
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 description 6
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 6
- 239000004215 Carbon black (E152) Substances 0.000 description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- 239000004793 Polystyrene Substances 0.000 description 6
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 6
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 6
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 6
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 6
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 6
- 125000002947 alkylene group Chemical group 0.000 description 6
- 229940018557 citraconic acid Drugs 0.000 description 6
- 230000007423 decrease Effects 0.000 description 6
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 6
- 238000011156 evaluation Methods 0.000 description 6
- 239000001530 fumaric acid Substances 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 229920000642 polymer Polymers 0.000 description 6
- 229920002223 polystyrene Polymers 0.000 description 6
- ARCGXLSVLAOJQL-UHFFFAOYSA-N trimellitic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C(C(O)=O)=C1 ARCGXLSVLAOJQL-UHFFFAOYSA-N 0.000 description 6
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 6
- 229920002554 vinyl polymer Polymers 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 229910001868 water Inorganic materials 0.000 description 6
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical group C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 5
- 239000005977 Ethylene Substances 0.000 description 5
- 150000008065 acid anhydrides Chemical class 0.000 description 5
- 150000007513 acids Chemical class 0.000 description 5
- 125000005907 alkyl ester group Chemical group 0.000 description 5
- 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 5
- 125000003118 aryl group Chemical group 0.000 description 5
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- 229910021506 iron(II) hydroxide Inorganic materials 0.000 description 5
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 description 5
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical class OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 4
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- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 4
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- 125000000217 alkyl group Chemical group 0.000 description 4
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 4
- HNEGQIOMVPPMNR-IHWYPQMZSA-N citraconic acid Chemical compound OC(=O)C(/C)=C\C(O)=O HNEGQIOMVPPMNR-IHWYPQMZSA-N 0.000 description 4
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- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 4
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Images
Abstract
【解決手段】結着樹脂及び磁性酸化鉄を少なくとも有する磁性トナーにおいて、該磁性酸化鉄の昇温酸化法によって得られるメインピーク温度が200℃以上400℃以下であり、昇温酸化法による測定で消費された酸素量が0.600mmol/g以上1.50mmol/g以下であり、該磁性酸化鉄のZn含有量が100ppm以下であることを特徴とする。
【選択図】なし
Description
該磁性酸化鉄の昇温酸化法によって得られるメインピーク温度が200℃以上400℃以下であり、昇温酸化法による測定で消費された酸素量が0.600mmol/g以上1.50mmol/g以下であり、該磁性酸化鉄のZn含有量が100ppm以下である磁性トナーに関する。
該静電荷像担持体のプロセススピードが500mm/sec以上800mm/sec以下であり、該磁性トナーが磁性酸化鉄の昇温酸化法によって得られるメインピーク温度が200℃以上400℃以下であり、昇温酸化法による測定で消費された酸素量が0.600mmol/g以上1.50mmol/g以下であり、該磁性酸化鉄のZn含有量が100ppm以下である磁性トナーであることを特徴とする画像形成方法に関する。
装置:BEL−CAT(触媒分析装置):日本ベル(株)社製
(i)前処理
試料(約0.2g)を付属のセルに秤量し、He雰囲気下(50ml/min),温度100℃で60分間前処理を行った。
(ii)分析条件
測定モード:TPO
キャリアガス濃度:酸素(4.91%)/He
開始温度:100℃
到達温度:1000℃
昇温速度:5℃/min
保持時間:20min
試料約1gに特級塩酸試薬16mlが溶解した塩酸水溶液26mlを加え粉末がなくなるまで加熱溶解、その後室温まで放冷する。特級フッ酸試薬2mlが溶解したフッ酸水溶液4ml添加後20分放置する。トリトンX(10%濃度)を10ml添加後10mlポリメスフラスコへ移し純粋を添加し全溶液を100mlに合わせる。
1.直径25mmのパラレルプレートを用いる。
2.周波数(Frequency)を0.1Hz(Initial),100Hz(Final)とする。
3.印加歪初期値(Strain)を0.1%に設定する。
4.スタート温度を100℃,終了温度を160℃,昇温ステップを10℃,保留時間(SOAK TIME)を1分とし測定を開始する。
5.自動テンションディレクション(Auto Tension Direction)をコンプレッション(Compression)と設定する。
6.初期スタティックフォース(Initial Static Force)を0g、自動テンションセンシティビティ(Auto Tension Sensitivity)を10.0gと設定する。
7.自動テンション(Auto Tension)の作動条件は、サンプルモデュラス(Sample Modulus)が1.0×106(Pa)よりも小さい場合である。
SiCl4+2H2+O2→SiO2+4HCl
温度40℃のヒートチャンバー中でカラムを安定化させ、この温度におけるカラムに溶媒としてTHFを毎分1mlの流速で流し、THF試料溶液を約100μl注入して測定する。試料の分子量測定にあたっては試料の有する分子量分布を数種の単分散ポリスチレン標準試料により作成された検量線の対数値とカウント値との関係から算出した。検量線作成用の標準ポリスチレン試料としては例えば、102以上107以下程度のものを用い、少なくとも10点程度の標準ポリスチレン試料を用いるのが適当である。例えば、東ソー社製TSK標準ポリスチレン(F−850,F−450,F−288,F−128,F−80,F−40,F−20,F−10,F−4,F−2,F−1,A−5000,A−2500,A−1000,A−500)を使用することが出来る。
測定装置:示差走査型熱量計(DSC)、MDSC−2920(TA Instruments社製)
ASTM D3418−82に準じて測定する。
試料0.900gを秤量し、1N−NaOH溶液25mlを加える。液を撹拌しながら45℃に加温し、粒子表面のケイ素成分やアルミニウム成分を溶解する(磁性酸化鉄中に含まれるケイ素成分やアルミニウム成分はアルカリ溶液には溶解してこない)。未溶解物を濾過した後、溶出液を純水で125mlに定量し、溶出液に含まれるケイ素やアルミニウムをプラズマ発光分析(ICP)で定量する。
表面被覆ケイ素成分、アルミニウム成分={溶出液に含まれるケイ素,アルミニウム(g/L)×125÷1000/0.900(g)}×100
プロポキシ化ビスフェノールA(2.2mol付加物) :24.5mol%
エトキシ化ビスフェノールA(2.2mol付加物) :25.5mol%
テレフタル酸 :33.0mol%
無水トリメリット酸 :5.0mol%
アジピン酸 :6.0mol%
アクリル酸 :4.0mol%
フマル酸 :2.0mol%
上記ポリエステルモノマーをエステル化触媒と共に4口フラスコに仕込み、減圧装置、水分離装置、窒素ガス導入装置、温度測定装置及び撹拌装置を装着して窒素雰囲気下にて温度135℃で撹拌した。本発明において所望の架橋構造を得るために本製造例においては反応の初期と後期にフマル酸を分割添加した。そこに、ビニル系共重合モノマー(スチレン:80mol%と2エチルヘキシルアクリレート:18mol%)と重合開始剤としてベンゾイルパーオキサイド2mol%を混合したものを滴下ロートから4時間かけて滴下した。その後、温度135℃で5時間反応した後、重縮合時の反応温度を230℃に昇温して縮重合反応を行った。反応終了後容器から取り出し、冷却、粉砕して結着樹脂1を得た。
<結着樹脂2の製造例>
テレフタル酸 31mol%
トリメリット酸 7mol%
プロポキシ化ビスフェノールA(2.2mol付加物) :33mol%
エトキシ化ビスフェノールA(2.2mol付加物) :29mol%
上記ポリエステルモノマーをエステル化触媒と共に4口フラスコに仕込み、減圧装置、水分離装置、窒素ガス導入装置、温度測定装置及び撹拌装置を装着して窒素雰囲気下にて温度135℃で撹拌した。そこに、ビニル系共重合モノマー(スチレン:83mol%と2エチルヘキシルアクリレート:15mol%)と重合開始剤としてベンゾイルパーオキサイド2mol%を混合したものを滴下ロートから4時間かけて滴下した。その後、温度135℃で5時間反応した後、重縮合時の反応温度を230℃に昇温して縮重合反応を行った。反応終了後容器から取り出し、冷却、粉砕して結着樹脂2を得た。
この結着樹脂2の諸物性については表1に示した通りである。
プロポキシ化ビスフェノールA(2.2mol付加物) :46.8mol%
テレフタル酸 :34.8mol%
無水トリメリット酸 :11.8mol%
イソフタル酸 :4.6mol%
フェノールノボラックEO付加物 :2.0mol%
上記のモノマーをエステル化触媒とともに5リットルオートクレーブに仕込み、還流冷却器、水分分離装置、N2ガス導入管,温度計及び撹拌装置を付し、オートクレーブ内にN2ガスを導入しながら温度230℃で重縮合反応を行った。反応終了後容器から取り出し、冷却、粉砕して結着樹脂3を得た。これらの樹脂の諸物性については表1に示した通りである。
プロポキシ化ビスフェノールA(2.2mol付加物) :45.1mol%
テレフタル酸 :51.9mol%
無水トリメリット酸 :3.0mol%
上記のモノマーをエステル化触媒とともに5リットルオートクレーブに仕込み、還流冷却器、水分分離装置、N2ガス導入管,温度計及び撹拌装置を付し、オートクレーブ内にN2ガスを導入しながら温度230℃で重縮合反応を行った。反応終了後容器から取り出し、冷却、粉砕して結着樹脂4を得た。これらの樹脂の諸物性については表1に示した通りである。
四つ口フラスコ内にキシレン300質量部を投入し、撹拌しながら容器内を充分に窒素で置換した後、昇温して還流させた。
四つ口フラスコ内にキシレン300質量部を投入し、撹拌しながら容器内を充分に窒素で置換した後、昇温して還流させた。
四つ口フラスコ内に、上記低分子量成分(5L)のキシレン溶液200質量部(低分子量成分30質量部相当)を投入し、昇温して還流下で撹拌する。一方、別容器に上記高分子量成分(5H)溶液200質量部(高分子量成分70質量部相当)を投入し、還流させる。上記低分子量成分(5L)溶液と高分子量成分(5H)溶液を還流下で混合した後、有機溶剤を留去し、得られた樹脂を冷却、固化後粉砕し結着樹脂5を得た。この結着樹脂の諸物性については表1に示した通りである。
Fe2+1.54mol/リットルを含む硫酸第一鉄水溶液65リットルと、2.38Nの水酸化ナトリウム水溶液88リットルを混合し、撹拌した。
磁性酸化鉄1の製造例に従い磁性酸化鉄2乃至4を製造した。尚、酸化反応により得られた磁性酸化鉄粒子を含むスラリーへのケイ酸ソーダの水溶液(Si品位13.4%)と硫酸アルミニウムの水溶液(Al品位4.2%)の投入量を調整することで被覆量を変化させた。磁性酸化鉄の諸物性については表2に示した通りである。
Fe2+1.54mol/リットルを含む硫酸第一鉄水溶液65リットルと、2.38Nの水酸化ナトリウム水溶液88リットルを混合し、撹拌した。
磁性酸化鉄5の製造例に従い磁性酸化鉄6乃至7を製造した。尚、酸化反応により得られた磁性酸化鉄粒子を含むスラリーへのケイ酸ソーダの水溶液(Si品位13.4%)と硫酸アルミニウムの水溶液(Al品位4.2%)の投入量を調整することで被覆量を変化させた。磁性酸化鉄の諸物性については表2に示した通りである。
2mol/リットルの硫酸第一鉄水溶液50リットルに、0.14mol/リットルの硫酸チタニル水溶液5リットルを、pH1.0、温度50℃の条件下で混合させ、十分撹拌した。このチタン塩含有硫酸第一鉄水溶液と、5mol/リットルの水酸化ナトリウム水溶液43リットルを混合し、水酸化第一鉄スラリーを得た。この水酸化第一鉄スラリーをpH12に維持し、温度85℃にて空気を吹き込み酸化反応を行った。その後、得られた磁性酸化鉄粒子を含むスラリーへケイ酸ソーダの水溶液(Si品位13.4%)を120g投入しpHを5以上9以下に調整し表面にケイ素を含む被覆層が形成された磁性酸化鉄スラリーを得た。このスラリーを常法により濾過、洗浄、乾燥、粉砕を行い、磁性酸化鉄粒子8を得た。磁性酸化鉄の諸物性については表2に示した通りである。
磁性酸化鉄粒子8の酸化反応後のスラリーを常法により濾過、洗浄、乾燥、粉砕を行い、磁性酸化鉄粒子9を得た。磁性酸化鉄の諸物性については表2に示した通りである。
Fe2+1.6mol/リットルを含む硫酸第一鉄水溶液21.0リットルと3.1Nの水酸化ナトリウム水溶液20.7リットルを混合し、撹拌した。その後、pH6.7,90℃で80l/minの空気を通気して第一段反応を開始し、同時にケイ素成分として3号水ガラス(SiO228.8wt%)196.3g(Feに対しSi換算で4.5原子%に該当する。)を水で希釈して0.3lとしたものを10分毎に0.06lづつ5回に分割して添加した。上記水ガラス溶液の滴下終了後、30分間撹拌しながら酸化反応を続け、第一段反応を終了させ磁性酸化鉄核晶粒子を含む第一鉄懸濁液を得た。このとき、酸化反応開始後、Fe2+の酸化度が20%を越えて以降のpHは7.5以上9.5以下の範囲内であり、しかも、30%を超えて以降のpHは8.0以上9.5以下の範囲内であった。第一段反応終了後の上記磁性酸化鉄核晶粒子を含む第一鉄塩懸濁液に9Nの水酸化ナトリウム水溶液0.4リットルを添加して懸濁液のpHを9.5に調整した後、温度90℃において100リットル/minの空気を30分間通気して第二段反応を行ってマグネタイト粒子を生成させた。生成粒子は、常法により、水洗、濾別、乾燥、粉砕した。磁性酸化鉄の諸物性については表2に示した通りである。
Fe2+1.54mol/リットルを含む硫酸第一鉄水溶液65リットルと、2.38Nの水酸化ナトリウム水溶液88リットルを混合し、撹拌した。
Fe2+を2.0mol/リットル含有する水溶液50リットルに水溶性ケイ酸塩としてSi4+を0.192mol/リットル含有する水溶液を20リットル添加し、NaOHを5.0mol/リットル含有する水溶液42リットルと撹拌混合した。得られたスラリー中の残留NaOHは2.5g/リットルであった。このスラリーの温度を85℃に維持しながら空気を65リットル/min通気することで酸化を行い、磁性酸化鉄コア粒子を含むスラリーを得た。
磁性酸化鉄12の製造例に従い磁性酸化鉄13を製造した。尚、酸化反応により得られた磁性酸化鉄粒子を含むスラリーへの硫酸亜鉛水溶液の投入量を調整することで亜鉛被覆量を変化させた。磁性酸化鉄の諸物性については表2に示した通りである。
・結着樹脂1 70質量部
・結着樹脂2 30質量部
・磁性酸化鉄粒子1 70質量部
・フィッシャートロプシュワックス(融点:101℃) 4質量部
・荷電制御剤−b−1 2質量部
上記材料をヘンシェルミキサーで前混合した後、二軸混練押し出し機によって、溶融混練した。
A(良):排紙接着が発生しない
B(可):紙同士の接着は見られるが剥がした際に画像に欠陥が見られることはない
C(悪い):剥がした際に画像に欠陥が見られる。
A(良):10%未満
B(可):10%以上、20%未満
C(悪い):20%以上
A:良好
B:わずかに汚れる程度
C:画像に影響する汚れ発生
表3に記載の処方で実施例1と同様に樹脂,荷電制御剤,磁性酸化鉄を変更し、磁性トナーNo2〜10を作製した。このようにして得られた物性値を表3に示し、同様の試験をした結果を表4,5,6,7に示す。
表3に記載の処方で実施例1と同様に樹脂,荷電制御剤,磁性酸化鉄を変更し、磁性トナーNo11〜16を作製した。このようにして得られた物性値を表3に示し、同様の試験をした結果を表4,5,6、7に示す。
Claims (5)
- 結着樹脂及び磁性酸化鉄を少なくとも含有する磁性トナー粒子を有する磁性トナーにおいて、
該磁性酸化鉄の昇温酸化法によって得られるメインピーク温度が200℃以上400℃以下であり、昇温酸化法による測定で消費された酸素量が0.600mmol/g以上1.50mmol/g以下であり、該磁性酸化鉄のZn含有量が100ppm以下であることを特徴とする磁性トナー。 - 該磁性酸化鉄を磁性トナー中に25質量%以上40質量%以下含有することを特徴とする請求項1に記載の磁性トナー。
- 該磁性トナーの粘弾性測定の周波数分散測定から得られる温度150℃を基準温度としたときのマスターカーブにおいて、シフトファクターaTから求められる活性化エネルギーEaが50kJ/mol以上120kJ/mol以下であることを特徴とする請求項1又は2に記載の磁性トナー。
- 少なくとも静電荷像を担持するための静電荷像担持体を帯電し、帯電された静電荷像担持体に静電荷像を形成し、静電荷像を現像スリーブ上の磁性トナーによって現像して磁性トナー像を形成し、静電荷像担持体上の磁性トナー像を中間転写材を介し、又は介さずに転写材へ転写し、転写材上の磁性トナー画像を熱定着手段によって定着する画像形成方法に使用される磁性トナーであって、
該静電荷像担持体のプロセススピードが500mm/sec以上800mm/sec以下であり、該磁性酸化鉄の昇温酸化法によって得られるメインピーク温度が200℃以上400℃以下であり、昇温酸化法による測定で消費された酸素量が0.600mmol/g以上1.50mmol/g以下であり、該磁性酸化鉄のZn含有量が100ppm以下であることを特徴とする磁性トナー。 - 少なくとも静電荷像を担持するための静電荷像担持体を帯電し、帯電された静電荷像担持体に静電荷像を形成し、静電荷像を現像スリーブ上の磁性トナーによって現像して磁性トナー像を形成し、静電荷像担持体上の磁性トナー像を中間転写材を介し、又は介さずに転写材へ転写し、転写材上の磁性トナー画像を熱定着手段によって定着する画像形成方法であって、
該静電荷像担持体のプロセススピードが500mm/sec以上800mm/sec以下であり、該磁性トナーが請求項1乃至3のいずれかに記載の磁性トナーであることを特徴とする画像形成方法。
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