JP2014160051A - カラム用コアシェル型粒子及びその製造方法 - Google Patents
カラム用コアシェル型粒子及びその製造方法 Download PDFInfo
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- JP2014160051A JP2014160051A JP2013098701A JP2013098701A JP2014160051A JP 2014160051 A JP2014160051 A JP 2014160051A JP 2013098701 A JP2013098701 A JP 2013098701A JP 2013098701 A JP2013098701 A JP 2013098701A JP 2014160051 A JP2014160051 A JP 2014160051A
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Landscapes
- Graft Or Block Polymers (AREA)
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Abstract
【解決手段】本発明は、親粒子と、該親粒子の外側に付着された複数の子粒子とを備えるカラム用コアシェル型粒子に関する。本発明はまた、親粒子と、該親粒子の外側に付着された複数の子粒子と、を備える、カラム用コアシェル型粒子の製造方法であって、官能基を有する親粒子の外側に高分子電解質を吸着させる工程と、上記高分子電解質の外側に子粒子を吸着させる工程とを含む、カラム用コアシェル型粒子の製造方法に関する。
【選択図】なし
Description
(GPC条件)
装置:(ポンプ:L−2130型(株式会社日立ハイテクノロジーズ製))、
(検出器:L−2490型RI(株式会社日立ハイテクノロジーズ製))、
(カラムオーブン:L−2350(株式会社日立ハイテクノロジーズ製))
カラム:Gelpack GL−R440 + Gelpack GL−R450
+ Gelpack GL−R400M(計3本)(日立化成(株)製、商品名)
カラムサイズ:10.7mmI.D×300mm
溶離液:テトラヒドロフラン
試料濃度:10mg/2mL
注入量:200μL
流量:2.05mL/分
測定温度:25℃
(1)官能基を有する親粒子を高分子電解質溶液に分散し、親粒子の表面に高分子電解質を吸着させた後、リンスする工程と、
(2)親粒子を子粒子の分散溶液に分散し、親粒子の表面に子粒子を吸着させた後、リンスする工程とを行うことで、表面に高分子電解質と子粒子とが積層された粒子を製造できる。
以下、本発明を実施例により説明するが、本発明はこれら実施例に限定されるものではない。
500mLの三口フラスコに、スチレン(ST)40g、オクタンチオール(OCT)4g、ペルオキソ二硫酸カリウム(KPS)1.98g及び水400gを一括して仕込み、70℃のウォーターバスで加熱しながら、攪拌機を用いて約8時間攪拌をして、種粒子を形成させた。種粒子は、平均粒子径0.75μm、粒径C.V.=2.3%、重量平均分子量Mw約25200であった。なお、粒子径測定はSEM(株式会社日立ハイテクノロジーズ製、製品名:S−4800)にて写真を撮像し、画像解析を行った。平均粒子径とC.V.の測定は、2000個の粒子で行った。以下同様である。
重合開始剤として過酸化ベンゾイル1g、モノマーとしてスチレン10g、ジビニルベンゼン2.5g、多孔質剤としてのトルエン3.75g、ジエチルベンゼン3.75g、カルボキシル基導入剤としてのメタクリル酸0.2gを溶媒(イオン交換水92.2質量%、エタノール7.5質量%に界面活性剤としてエマールTD(ラウリル硫酸トリエタノールアミン、花王株式会社製、商品名(「エマール」は、登録商標。))0.3質量%純水)340gに分散し、ホモジナイザーで10分間超音波照射し、乳化を行った。その後、種粒子1を固形分で0.70g添加した後、20時間膨潤を行った。その後80℃に昇温し、8時間重合を行った。重合終了後、得られた粒子を、水、メタノールで洗浄を行った。合成した粒子は、平均粒子径4.05μm、粒径C.V.=3.3%であった。
メタクリル酸0.2gを入れなかったこと以外は多孔質親粒子1と同様に多孔質粒子2の合成を行った。
純水400g中に表1の子粒子1〜6の配合表にしたがって材料を添加し、攪拌速度200min−1で攪拌しながら、80℃、6時間加熱を行った。合成した粒子をSEM(S−4800)にて写真を撮像し、画像解析を行った。平均粒子径測定は100個の粒子で行った。以下同様である。子粒子の形状は、赤血球形状、ジャガイモ状(表面がでこぼこ状)、球状のいずれかであった。
次に、重量平均分子量70,000の30質量%ポリエチレンイミン水溶液(和光純薬工業株式会社製)を超純水で希釈し、0.3質量%ポリエチレンイミン水溶液を得た。前記カルボキシル基を有する多孔質粒子1を10g、前記0.3質量%ポリエチレンイミン水溶液に加え、室温で15分攪拌した。次に、孔径3μmのメンブレンフィルタ(ミリポア社製)で多孔質粒子をろ過し、超純水200gに入れて室温で5分間攪拌した。更に孔径3μmのメンブレンフィルタ(ミリポア社製)で多孔質粒子をろ過し、前記メンブレンフィルタ上にて200gの超純水で2回洗浄して、吸着していないポリエチレンイミンを除去することで、表面にアミノ基含有ポリマーを有する多孔質粒子を作製した。
子粒子1の代わりに子粒子2を用いた以外はカラム用コアシェル型粒子1と同様の方法でカラム用コアシェル型粒子2を作製した。
子粒子1の代わりに子粒子3を用いた以外はカラム用コアシェル型粒子1と同様の方法でカラム用コアシェル型粒子3を作製した。
子粒子1の代わりに子粒子4を用いた以外はカラム用コアシェル型粒子1と同様の方法でカラム用コアシェル型粒子4を作製した。
子粒子1の代わりに子粒子5を用いた以外はカラム用コアシェル型粒子1と同様の方法でカラム用コアシェル型粒子5を作製した。
子粒子1の代わりに子粒子6を用いた以外はカラム用コアシェル型粒子1と同様の方法でカラム用コアシェル型粒子6を作製した。
子粒子被覆率が10%となるようにした以外はカラム用コアシェル型粒子1と同様の方法でカラム用コアシェル型粒子7を作製した。
子粒子被覆率が60%となるようにした以外はカラム用コアシェル型粒子1と同様の方法でカラム用コアシェル型粒子8を作製した。
多孔質親粒子1の代わりに多孔質親粒子2を用いた以外はカラム用コアシェル型粒子1と同様の方法でカラム用コアシェル型粒子9を作製した。
10gの多孔質親粒子1に対し、ジクロロエタン57g、97質量%硫酸92gを加え、110℃で4時間反応を行い、スルホン酸基を導入した多孔質ポリマー粒子を合成した。その後、80℃、1時間の条件で加熱乾燥を行うことで通常粒子を作製した。
直径7.8mm、長さ150mmのステンレスカラムに、充填溶媒0.1質量%リン酸、スラリー濃度50質量%、充填圧15MPa、充填時間30分間の条件で充填した。
充填したカラムを用い、高速液体クロマトグラフ(L2000、株式会社日立ハイテクノロジーズ製)にて、溶離液0.1質量%リン酸水溶液、カラム温度25℃、流速0.5mL/分、サンプル3.5質量%蟻酸、サンプル注入量2μL、溶出器UV210nmの測定条件でクロマト特性を測定した。クロマト測定により、理論段数、カラム圧、ピーク対称度、ピーク形状を求め、粒子特性の指標とした。
実験結果を表2に示す。なお、表2に示す子粒子の被覆率は、実験終了後、カラムから粒子を100個取り出してSEM画像解析により、(絶縁被覆部分の表面積/全体の表面積)×100%で算出した。
Claims (10)
- 親粒子と、該親粒子の外側に付着された複数の子粒子とを備える、カラム用コアシェル型粒子。
- 前記子粒子が、前記親粒子の外側に化学結合して付着される、請求項1に記載のカラム用コアシェル型粒子。
- 前記子粒子が、前記親粒子の外側に高分子を介して化学結合して付着される、請求項2に記載のカラム用コアシェル型粒子。
- 前記子粒子の被覆率が、前記親粒子の総表面積に対して10〜70%の範囲である、請求項1〜3のいずれか一項に記載のカラム用コアシェル型粒子。
- 前記子粒子が、半円型の粒子である、請求項1〜4のいずれか一項に記載のカラム用コアシェル型粒子。
- 前記子粒子が、表面に凸凹を有する球状の粒子である、請求項1〜4のいずれか一項に記載のカラム用コアシェル型粒子。
- 親粒子と、該親粒子の外側に付着された複数の子粒子と、を備えるカラム用コアシェル型粒子の製造方法であり、
官能基を有する親粒子の外側に高分子電解質を吸着させる工程と、
前記高分子電解質の外側に子粒子を吸着させる工程とを含む、
カラム用コアシェル型粒子の製造方法。 - 前記官能基がカルボキシル基である、請求項7に記載のカラム用コアシェル型粒子の製造方法。
- 前記高分子電解質がポリアミンである、請求項7又は8に記載のカラム用コアシェル型粒子の製造方法。
- 前記高分子電解質がポリエチレンイミンである、請求項7〜9のいずれか一項に記載のカラム用コアシェル型粒子の製造方法。
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