JP6245769B2 - 荷電制御剤、及び荷電制御剤を含む静電荷像現像用トナー - Google Patents
荷電制御剤、及び荷電制御剤を含む静電荷像現像用トナー Download PDFInfo
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- JP6245769B2 JP6245769B2 JP2016206546A JP2016206546A JP6245769B2 JP 6245769 B2 JP6245769 B2 JP 6245769B2 JP 2016206546 A JP2016206546 A JP 2016206546A JP 2016206546 A JP2016206546 A JP 2016206546A JP 6245769 B2 JP6245769 B2 JP 6245769B2
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- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 claims description 10
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- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 claims description 8
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Description
(1. 荷電制御剤Aの調製)
荷電制御剤Aを以下のようにして調製した。
(1) 反応工程(モノアゾ化合物の合成)
濃塩酸95kgを水150Lで希釈し、これに2−アミノ−4−tert−ブチルフェノール45kgを投入して溶解後、氷150kgで5℃まで冷却した。これに40%亜硝酸ナトリウム水溶液49kgを徐々に加えてジアゾ化反応を行い、ジアゾニウム塩を得た。別に、ナフトールAS70kgと48%水酸化カリウム水溶液60kgとを水280Lに加えて溶解させた。これに、ジアゾニウム塩溶液とn−ブタノール40kgとを滴下し、80℃で2時間反応した。反応後、遠心分離機で濾過・水洗してモノアゾ化合物のウエットケーキ275kgを得た。
反応工程で得られたモノアゾ化合物のウエットケーキ全量を水1000Lに加え、48%水酸化カリウム水溶液90kgとn−ブタノール80kgとを加えて80℃で分散した。分散後40%硫酸第二鉄水溶液130kgを滴下した。この時の反応液のpHは2.8であった。80℃で6時間反応を行い、アゾ鉄錯塩を得た。反応後、プレスフィルターで濾過・水洗してアゾ系鉄錯塩のウエットケーキ312kgを得た。
金属化工程で得られたアゾ系鉄錯塩のウエットケーキ全量をパドル乾燥機(株式会社ネオテック製、製品名:PD−1500V)に投入し、パドル乾燥機の処理室の圧力を60mmHgに減圧した。蒸気圧0.1MPaの蒸気をパドル乾燥機のジャケットに導入して循環させることによって、パドル乾燥機の処理室を70℃まで昇温した。この温度に達した時から6時間までの前半は、パドル乾燥機の回転軸を4rpmで回転させてウエットケーキを乾燥させた。このとき大部分の水が留去されるまで、処理室を100mmHg〜200mmHgに保った。6時間経過後の後半は、蒸気圧を0.55MPaに昇圧して処理室を120℃とし、さらに24時間撹拌することにより、荷電制御剤Aを調製した。
(測定1)平均粒径の測定
凝集粒子である荷電制御剤A5mgを、活性剤(花王株式会社製、製品名:モア)5v/v%の溶液に加え混合液とし、5分間超音波振動させた。この混合液0.25mLを、粒度分布測定器(株式会社堀場製作所製、製品名:LA−950)に投入し、さらに5分間超音波振動させ微細分散させた後、粒度分布を測定した。D10値は体積基準における累積頻度が10%を示す時の粒子径、D50値は体積基準における累積頻度が50%を示す時の粒子径(メジアン径)を表す。荷電制御剤AのD10値は0.89μm、D50値は1.56μmであった。
水素イオン量、Naイオン量及びKイオン量の測定
原子吸光測定器(バリアン テクノロジーズ ジャパン リミテッド社製、製品名:SpectrAA−220FS)を用い、荷電制御剤A中のNaとK含有量を測定した結果、対イオンとしての存在モル%比率は水素イオンが99.7%であり、Naイオン量が0%、Kイオン量が0.3%であった。
荷電制御剤A5gを100mLのイオン交換水に分散し、その際の重量を記録した。これを、イオン成分を抽出するために煮沸抽出し、抽出後に濾過した。濾液の重量を初期の重量と同じになるまでイオン交換水を加え、この溶液のpHをpHメーター(東亜ディーケーケー株式会社製、製品名:HM30R)で測定した結果、荷電制御剤AのpHは6.2であった。
荷電制御剤A5gを500mLのイオン交換水に分散し、その際の重量を記録した。これを、イオン成分を抽出するために煮沸抽出し、抽出後に濾過した。濾液の重量を初期の重量と同じになるまでイオン交換水を加え、この溶液の電気伝導度を電気伝導率計(東亜ディーケーケー株式会社製、製品名:AOL−10)で測定した結果、荷電制御剤Aの電気伝導度は167μS/cmであった。
荷電制御剤A2gを秤量瓶(重量a)に加え、全重量(重量b)を測定した。秤量瓶を107℃に保持した温風乾燥機中に入れ、2時間放置後、乾燥剤を入れたデシケーター中で室温まで放冷した。放冷後に秤量瓶の重量(重量c)を測定し、
揮発成分(%)={(b−a)-(c−a)}/(b−a)×100
の計算式で揮発成分を求めた結果、荷電制御剤Aの揮発成分は0.23%であった。
荷電制御剤A1gをるつぼ(重量a)に入れ、全重量(重量b)を測定した。るつぼを800℃に保持した電気炉中に入れ、2時間放置後、乾燥剤を入れたデシケーター中で室温まで放冷した。放冷後にるつぼの重量(重量c)を測定し、
灰分(%)=(c−a)/(b−a)×100
の計算式で灰分を求めた結果、荷電制御剤Aの灰分は8.72%であった。
粉末X線回折パターンを以下の条件で測定した。
使用装置:X線回折装置(株式会社リガク製、製品名:RINT TTRIII)
X線源:Cu
管電圧,管電流:50.0kV,300mA
発散スリット:2/3°
受光スリット:0.30mm
散乱スリット:2/3°
走査速度:4.0°/min
サンプリング幅:0.02°
走査範囲:5.0〜40.0°
ピークサーチ条件:二次微分法、ピーク幅閾値0.2°、ピーク強度閾値600cps
調製実施例1の乾燥工程の前半において、乾燥時間を10時間としたこと以外は、調製実施例1と同様にして荷電制御剤Bを調製した。得られた荷電制御剤BのX線回折を測定すると、6.6°、10.3°、18.3°、19.5°、21.7°に主要なピークとともに、31.7°にピークが確認された。
調製実施例2の乾燥工程の前半において、処理室の圧力を30mmHgとしたこと以外は、調製実施例2と同様にして荷電制御剤Cを調製した。得られた荷電制御剤CのX線回折を測定すると、6.6°、10.3°、18.3°、19.5°、21.7°に主要なピークとともに、31.7°にピークが確認された。
調製実施例1の乾燥工程の後半において、蒸気圧を0.6MPaとしたこと以外は、調製実施例1と同様にして荷電制御剤Dを調製した。得られた荷電制御剤DのX線回折を測定すると、6.6°、10.3°、18.3°、19.5°、21.7°に主要なピークとともに、31.7°にピークが確認された。
調製実施例2の乾燥工程の後半において、48時間継続したこと以外は、調製実施例2と同様にして荷電制御剤Eを調製した。得られた荷電制御剤EのX線回折を測定すると、6.6°、10.3°、18.3°、19.5°、21.7°に主要なピークとともに、31.7°にピークが確認された。
(1) モノアゾ化合物の合成
濃塩酸95kgを水150Lで希釈し、これに2−アミノ−4−tert−ブチルフェノール45kgを投入して溶解後、氷150kgで5℃まで冷却した。これに40%亜硝酸ナトリウム水溶液49kgを徐々に加えてジアゾ化反応を行い、ジアゾニウム塩を得た。別に、ナフトールAS70kgと48%水酸化カリウム水溶液60kgとを水280Lに加えて溶解させた。これに、ジアゾニウム塩溶液とイソブタノール40kgとを滴下し、80℃で2時間反応した。反応後、遠心分離機で濾過・水洗してウエットケーキ281kgを得た。
得られたモノアゾ化合物のウエットケーキ全量を水1000Lに加え、48%水酸化カリウム水溶液90kgとイソブタノール80kgとを加えて80℃で分散した。分散後40%硫酸第二鉄水溶液130kgを滴下した。この時の反応液のpHは2.6であった。80℃で6時間反応を行い、アゾ鉄錯塩を得た。反応後、プレスフィルターで濾過・水洗してウエットケーキ309kgを得た。
得られたウエットケーキ全量を金属トレイに移した後に棚型温風乾燥機に投入し、庫内温度120℃で24時間乾燥することにより、荷電制御剤Fを調製した。
スチレン−アクリル共重合樹脂(三井化学株式会社製、製品名:CPR−100)を100重量部と、低分子量ポリプロピレン(三洋化成工業株式会社製、製品名:ビスコール550−P)を2重量部と、カーボンブラック(三菱化学株式会社製、製品名:MA100)を6重量部と、荷電制御剤Aを1重量部とを高速ミキサーで均一にプレミキシングした。次いで、ニーダー(株式会社栗本鐵工所製、製品名:S1KRC2軸混練押出機)で溶融混練(温度130℃)し、冷却後、ローターミル(Retsch社製、製品名:ZM1)で粗粉砕した。得られた粗砕物を分級機付きのエアージェットミル(セイシン企業株式会社製、製品名:CO−JET Systemα)を用いて微粉砕して、粒径10μmのトナーを得た。
{[(標準条件下の帯電量)−(低温低湿下の帯電量)]/(標準条件下の帯電量)}×100
及び
{[(標準条件下の帯電量)−(高温高湿下の帯電量)]/(標準条件下の帯電量)}×100
の式に従って値を求め、その変化率の絶対値が0.0〜5.0%であったものを○、5.0〜10.0%であったものを△、10.0%以上のものを×とする3段階で評価した。結果を表3に示す。
Claims (3)
- 下記化学式(3)
で表されるアゾ系鉄錯塩を含み、CuKα特性X線によるX線回折スペクトルのピークを、ブラッグ角2θにおいて少なくとも6.6±0.2°、10.3±0.2°、18.3±0.2°、19.5±0.2°、21.7±0.2°、及び31.7±0.2°に有し、レーザー回折散乱式粒度分布測定方法によって測定された前記アゾ系鉄錯塩の体積基準における粒径の累積頻度が、10%で0.6〜1.1μmであり、50%で1.3〜1.8μmであることを特徴とする荷電制御剤。 - 前記アゾ系鉄錯塩の揮発成分が、0.1〜0.7重量%である請求項1に記載の荷電制御剤。
- 請求項1又は2に記載の荷電制御剤と、トナー用樹脂とが、含まれていることを特徴とする静電荷像現像用トナー。
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