JP2004245825A - トナー濃度定量方法およびトナー含有ポリエステルの製造方法 - Google Patents
トナー濃度定量方法およびトナー含有ポリエステルの製造方法 Download PDFInfo
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- JP2004245825A JP2004245825A JP2004000912A JP2004000912A JP2004245825A JP 2004245825 A JP2004245825 A JP 2004245825A JP 2004000912 A JP2004000912 A JP 2004000912A JP 2004000912 A JP2004000912 A JP 2004000912A JP 2004245825 A JP2004245825 A JP 2004245825A
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- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 description 1
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 description 1
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Landscapes
- Investigating Or Analysing Materials By Optical Means (AREA)
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Abstract
【解決手段】(1)トナー分散液中のトナー濃度を定量するに当たり、トナー分散液と有機溶媒とを接触させて有機溶媒でトナーを抽出し、得られた抽出溶液の吸光度を測定する。(2)トナー分散液調製工程、反応系にトナー分散液を混合する工程、エステル化またはエステル交換反応工程、重縮合工程を含むトナー含有ポリエステルの製造方法に於いて、反応系にトナー分散液を混合する工程を行なうに際し、上記の(1)に記載の方法でトナー分散液中のトナー濃度を定量し、その結果に基づき、生成ポリマーに対するトナー添加量が所定の量となる様にトナー分散液の供給量および/またはトナー分散液調製濃度をコントロールする。
【選択図】 なし
Description
凍結粉砕した樹脂粒状体ポリエステルペレット試料0.50gを、フェノール/1,1,2,2−テトラクロロエタン(重量比1/1)の混合溶媒に溶解させて濃度(c)1.0g/dlの溶液を調製した。この際、溶融重合樹脂の場合は110℃で20分かけて溶解し、固相重合樹脂の場合は120℃で20分かけて溶解した。その後、ウベローデ型毛細粘度管を使用し、30℃で、原液との相対粘度(ηrel)を測定し、この相対粘度(ηrel)−1から求めた比粘度(ηsp)と濃度(c)との比(ηsp/c)を求めた。同様の方法により、濃度(c)が0.5g/dl、0.2g/dl、0.1g/dlの各場合についても比(ηsp/c)を求めた。そして、これらの値より、濃度(c)を0に外挿したときの比(ηsp/c)を固有粘度〔η〕(dl/g)として求めた。
内径36mm、深さ15mmの円柱状の粉体測色用セルに、樹脂粒状体試料をすりきりに充填し、測色色差計(日本電色工業社製「ND−300A」)を使用し、JIS Z8730の参考1に規定される、Lab表色系によるハンターの色差式の色座標bを、反射法により、測定セルを90度ずつ回転させて4箇所測定した値の単純平均値として求めた。色座標b値はマイナスになるほど青味が強く、逆に、プラスになるほど黄味が強い色調を表す。
トナー(有機系調色剤)として、カラーインデックスで、ソルベントブルー104(クラリアント社製「Polysynthren Blue RBL」使用。以下、「S.B.104」と略す。)とソルベントレッド135(クラリアント社製「Sandoplast Red G」使用。以下、「S.R.135」と略す。)を使用した。分液ロートに、上記のトナーの混合エチレングリコール分散液1mLとクロロホルム30mLを添加し、よく振り混ぜてトナーをクロロホルム相へ抽出した。抽出溶液(クロロホルム相)を採取し、分光光度計にて450nmと632nmの吸光度を測定し、後述する検量式よりトナー濃度を定量した。
分液ロートに、「S.B.104」/「S.R.135」混合エチレングリコールスラリー分散液(調製濃度0.050/0.050w%)1mLとクロロホルム30mLを添加し、よく振り混ぜてトナーをクロロホルム相に抽出した。抽出溶液(クロロホルム相)を採取し、分光光度計にて450nmと632nmの吸光度を測定した。
<トナー濃度の定量>
「S.B.104」/「S.R.135」混合エチレングリコール分散液0.074/0.102wt%を調製し(分散液A)、分液ロートに分散液A1mLとクロロホルム30mLを添加し、よく振り混ぜてトナーをクロロホルム相に抽出した。抽出溶液(クロロホルム相)を採取し、分光光度計にて450nmと632nmの吸光度を測定し、前記の検量式より濃度を定量した。その結果を表1に示す。
実施例1において、抽出操作を省略し、分散液A(エチレングリコール分散液)のまま吸光度を測定した。その結果を表2に示す。
実施例2
スラリー調製槽、それに直列に接続された2段のエステル化反応槽、2段目のエステル化反応槽に直列に接続された3段の溶融重縮合槽から成る連続重合装置を使用し、スラリー調製槽に、テレフタル酸とエチレングリコールを重量比で8W65:485の割合で連続的に供給すると共に、エチルアシッドホスフェートの0.6重量%エチレングリコール溶液を、得られるポリエステル樹脂1トン当たりのリン原子としての総量Pが0.129モル/樹脂トンとなる量で連続的に添加し、且つ、トナー分散液調製槽にて調製した「S.B.104」/「S.R.135」混合エチレングリコール分散液(調製濃度0.10/0.10wt%)を、得られるポリエステル樹脂1トン当たりのトナーの総量が1.0g/樹脂トンとなる量で連続的に添加した。
実施例2において、「S.B.104」/「S.R.135」0.1/0.1wt%混合エチレングリコール分散液を、得られるポリエステル樹脂1トン当たりのトナーの総量が1.0g/樹脂トンとなる様に調製濃度から計算して連続的に添加したこと以外は、同様の方法にてポリエステル樹脂を製造した。この樹脂のカラーb値を表5に示す。
Claims (7)
- トナー分散液中のトナー濃度を定量するに当たり、トナー分散液と有機溶媒とを接触させて有機溶媒でトナーを抽出し、得られた抽出溶液の吸光度を測定することを特徴とするトナー濃度定量方法。
- トナーが、アントラキノン系化合物およびペリノン系化合物の群から選択される1種または2種以上である請求項1に記載のトナー濃度定量方法。
- トナーが、カラーインデックスのソルベントブルー97、ソルベントブルー104、ソルベントレッド135、ソルベントレッド179の群から選択される1種または2種以上である請求項1又は2に記載のトナー濃度定量方法。
- 分散媒がエチレングリコール及び/又は水である請求項1〜3の何れかに記載のトナー濃度定量方法。
- トナーの抽出に使用する有機溶媒がクロロホルム又はトルエンである請求項1〜4の何れかに記載のトナー濃度定量方法。
- トナー分散液調製工程、反応系にトナー分散液を混合する工程、エステル化またはエステル交換反応工程、重縮合工程を含むトナー含有ポリエステルの製造方法に於いて、反応系にトナー分散液を混合する工程を行なうに際し、請求項1に記載の方法でトナー分散液中のトナー濃度を定量し、その結果に基づき、生成ポリマーに対するトナー添加量が所定の量となる様にトナー分散液の供給量および/またはトナー分散液調製濃度をコントロールすることを特徴とするトナー含有ポリエステルの製造方法。
- ポリエステルがチタンを含んでいる請求項6に記載のトナー含有ポリエステルの製造方法。
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JP4750221B1 (ja) * | 2010-11-18 | 2011-08-17 | マークテック株式会社 | 湿式蛍光磁粉探傷試験に用いる検査液における各成分濃度の測定方法および測定装置 |
WO2011138843A1 (ja) * | 2010-05-07 | 2011-11-10 | マークテック株式会社 | 湿式蛍光磁粉探傷試験に用いる検査液における成分濃度の測定方法および測定装置 |
JP2011237227A (ja) * | 2010-05-07 | 2011-11-24 | Marktec Corp | 湿式蛍光磁粉探傷試験に用いる検査液における成分濃度の測定方法および測定装置 |
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WO2011138843A1 (ja) * | 2010-05-07 | 2011-11-10 | マークテック株式会社 | 湿式蛍光磁粉探傷試験に用いる検査液における成分濃度の測定方法および測定装置 |
JP2011237227A (ja) * | 2010-05-07 | 2011-11-24 | Marktec Corp | 湿式蛍光磁粉探傷試験に用いる検査液における成分濃度の測定方法および測定装置 |
JP4750221B1 (ja) * | 2010-11-18 | 2011-08-17 | マークテック株式会社 | 湿式蛍光磁粉探傷試験に用いる検査液における各成分濃度の測定方法および測定装置 |
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