JP7443330B2 - 吸水性樹脂粒子及びその製造方法、吸収体、吸収性物品、並びに、浸透速度の調整方法 - Google Patents
吸水性樹脂粒子及びその製造方法、吸収体、吸収性物品、並びに、浸透速度の調整方法 Download PDFInfo
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- JP7443330B2 JP7443330B2 JP2021505001A JP2021505001A JP7443330B2 JP 7443330 B2 JP7443330 B2 JP 7443330B2 JP 2021505001 A JP2021505001 A JP 2021505001A JP 2021505001 A JP2021505001 A JP 2021505001A JP 7443330 B2 JP7443330 B2 JP 7443330B2
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Description
(1)前記吸水性樹脂粒子1質量部及び水199質量部を混合することによりゲルを得る。
(2)ロートにおける直径8mmの円形の下端開口を閉止した状態で前記ロートに前記ゲルを収容する。
(3)前記下端開口を開放して3分経過したときの前記ゲルの単位時間あたりの流出量を前記ゲルフローレートとして測定する。
(1)前記吸水性樹脂粒子1質量部及び水199質量部を混合することによりゲルを得る。
(2)ロートにおける直径8mmの円形の下端開口を閉止した状態で前記ロートに前記ゲルを収容する。
(3)前記下端開口を開放して3分経過したときの前記ゲルの単位時間あたりの流出量を前記ゲルフローレートとして測定する。
(1)前記吸水性樹脂粒子1質量部及び水199質量部を混合することによりゲルを得る。
(2)ロートにおける直径8mmの円形の下端開口を閉止した状態で前記ロートに前記ゲルを収容する。
(3)前記下端開口を開放して3分経過したときの前記ゲルの単位時間あたりの流出量を前記ゲルフローレートとして測定する。
(1)前記吸水性樹脂粒子1質量部及び水199質量部を混合することによりゲルを得る。
(2)ロートにおける直径8mmの円形の下端開口を閉止した状態で前記ロートに前記ゲルを収容する。
(3)前記下端開口を開放して3分経過したときの前記ゲルの単位時間あたりの流出量を前記ゲルフローレートとして測定する。
含水率=[Ww/(Ww+Ws)]×100
Ww:全重合工程の重合前の単量体水溶液に含まれる水分量から、乾燥工程により系外部に排出された水分量を差し引いた量に、凝集剤、表面架橋剤等を混合する際に必要に応じて用いられる水分量を加えた含水ゲル状重合体の水分量。
Ws:含水ゲル状重合体を構成するエチレン性不飽和単量体、架橋剤、開始剤等の材料の仕込量から算出される固形分量。
(実施例1)
還流冷却器、滴下ロート、窒素ガス導入管、及び、撹拌機を備えた内径11cm、内容積2Lの丸底円筒型セパラブルフラスコを準備した。撹拌機には、図2に概形を示す撹拌翼(平板翼)200を取り付けた。撹拌翼200は、軸200a及び平板部200bを備えている。平板部200bは、軸200aに溶接されていると共に、湾曲した先端を有している。平板部200bには、軸200aの軸方向に沿って延びる4つのスリットSが形成されている。4つのスリットSは平板部200bの幅方向に配列されており、内側の二つのスリットSの幅は1cmであり、外側二つのスリットSの幅は0.5cmである。平板部200bの長さは約10cmであり、平板部200bの幅は約6cmである。続いて、上述のセパラブルフラスコに、炭化水素分散媒としてn-ヘプタン293gを添加し、高分子系分散剤として無水マレイン酸変性エチレン・プロピレン共重合体(三井化学株式会社製、ハイワックス1105A)0.736gを添加することにより混合物を得た。この混合物を撹拌しつつ80℃まで昇温することにより分散剤を溶解した後、混合物を50℃まで冷却した。
第2段目の重合後の含水ゲル状重合体において、共沸蒸留により224.3gの水を系外へ抜き出したこと以外は、実施例1と同様にして、吸水性樹脂粒子231.0gを得た。吸水性樹脂粒子の中位粒子径は342μmであった。
第2段目の重合後の含水ゲル状重合体において、共沸蒸留により234.6gの水を系外へ抜き出したこと以外は、実施例1と同様にして、吸水性樹脂粒子232.1gを得た。吸水性樹脂粒子の中位粒子径は355μmであった。
無水マレイン酸変性エチレン・プロピレン共重合体を溶解させる際に、撹拌機として、平板翼に代えて、翼径5cmの4枚傾斜パドル翼を2段有する撹拌翼を用いたこと、第1段目の水性液の調製において、水溶性ラジカル重合開始剤として2,2’-アゾビス(2-アミジノプロパン)2塩酸塩を用いずに、過硫酸カリウム0.0736g(0.272ミリモル)を用いると共に、内部架橋剤としてエチレングリコールジグリシジルエーテル0.010g(0.057ミリモル)を用いたこと、第1段目の重合スラリー液の調製において撹拌機の回転数を550rpmへ変更したこと、第2段目の水性液の調製において、水溶性ラジカル重合開始剤として2,2’-アゾビス(2-アミジノプロパン)2塩酸塩を用いずに、過硫酸カリウム0.090g(0.333ミリモル)を用いると共に内部架橋剤としてエチレングリコールジグリシジルエーテル0.0117g(0.067ミリモル)を用いたこと、第2段目の水性液の全量を第1段目の重合スラリー液に添加する際の撹拌機の回転数を1000rpmへ変更したこと、第2段目の重合後の含水ゲル状重合体に添加する45質量%のジエチレントリアミン5酢酸5ナトリウム水溶液の使用量を0.265gへ変更すると共に、共沸蒸留により247.9gの水を系外へ抜き出したこと、及び、重合体粒子の質量に対して0.5質量%の非晶質シリカを重合体粒子と混合したこと以外は、実施例1と同様にして、吸水性樹脂粒子231.0gを得た。吸水性樹脂粒子の中位粒子径は355μmであった。
第2段目の重合後の含水ゲル状重合体において、共沸蒸留により253.9gの水を系外へ抜き出したこと、及び、重合体粒子の質量に対して0.1質量%の非晶質シリカを重合体粒子と混合したこと以外は、比較例1と同様にして、吸水性樹脂粒子230.8gを得た。吸水性樹脂粒子の中位粒子径は360μmであった。
第2段目の重合後の含水ゲル状重合体において、共沸蒸留により271.4gの水を系外へ抜き出したこと、及び、当該共沸蒸留の後に添加する2質量%のエチレングリコールジグリシジルエーテル水溶液の使用量を6.40g(0.735ミリモル)へ変更したこと以外は、比較例1と同様にして、吸水性樹脂粒子230.6gを得た。吸水性樹脂粒子の中位粒子径は355μmであった。
第2段目の重合後の含水ゲル状重合体において、共沸蒸留により278.9gの水を系外へ抜き出したこと、及び、重合体粒子の質量に対して0.2質量%の非晶質シリカを重合体粒子と混合したこと以外は、比較例1と同様にして、吸水性樹脂粒子230.8gを得た。吸水性樹脂粒子の中位粒子径は358μmであった。
還流冷却器、滴下ロート、窒素ガス導入管、及び、撹拌機(翼径5cmの4枚傾斜パドル翼を2段有する撹拌翼)を備えた内径11cm、内容積2Lの丸底円筒型セパラブルフラスコを準備した。このフラスコに、炭化水素分散媒としてn-ヘプタン300gを添加し、高分子系分散剤として無水マレイン酸変性エチレン・プロピレン共重合体(三井化学株式会社製、ハイワックス1105A)0.74gを添加することにより混合物を得た。この混合物を撹拌しつつ分散剤を加温溶解した後、混合物を50℃まで冷却した。
吸水性樹脂粒子の上述の中位粒子径は下記手順により測定した。すなわち、JIS標準篩を上から、目開き600μmの篩、目開き500μmの篩、目開き425μmの篩、目開き300μmの篩、目開き250μmの篩、目開き180μmの篩、目開き150μmの篩、及び、受け皿の順に組み合わせた。組み合わせた最上の篩に、吸水性樹脂粒子50gを入れ、ロータップ式振とう器(株式会社飯田製作所製)を用いてJIS Z 8815(1994)に準じて分級した。分級後、各篩上に残った粒子の質量を全量に対する質量百分率として算出し粒度分布を求めた。この粒度分布に関して粒子径の大きい方から順に篩上を積算することにより、篩の目開きと篩上に残った粒子の質量百分率の積算値との関係を対数確率紙にプロットした。確率紙上のプロットを直線で結ぶことにより、積算質量百分率50質量%に相当する粒子径を中位粒子径として得た。
吸水性樹脂粒子の生理食塩水の保水量(室温、25±2℃)を下記手順で測定した。まず、吸水性樹脂粒子2.0gを量り取った綿袋(メンブロード60番、横100mm×縦200mm)を内容積500mLのビーカー内に設置した。吸水性樹脂粒子の入った綿袋内に生理食塩水500gを、ママコができないように一度に注ぎ込んだ後、綿袋の上部を輪ゴムで縛り、30分静置させることで吸水性樹脂粒子を膨潤させた。30分経過後の綿袋を、遠心力が167Gとなるように設定した脱水機(株式会社コクサン製、品番:H-122)を用いて1分間脱水した後、脱水後の膨潤ゲルを含んだ綿袋の質量Wa[g]を測定した。吸水性樹脂粒子を添加せずに同様の操作を行い、綿袋の湿潤時の空質量Wb[g]を測定し、下記式から吸水性樹脂粒子の生理食塩水の保水量を算出した。結果を表1に示す。
保水量[g/g]=(Wa-Wb)/2.0
吸水性樹脂粒子の荷重下の生理食塩水の吸水量(室温、25℃±2℃)を、図3に示す測定装置Yを用いて測定した。測定装置Yは、ビュレット部61、導管62、測定台63、及び、測定台63上に置かれた測定部64から構成される。ビュレット部61は、鉛直方向に伸びるビュレット61aと、ビュレット61aの上端に配置されたゴム栓61bと、ビュレット61aの下端に配置されたコック61cと、コック61cの近傍において一端がビュレット61a内に伸びる空気導入管61dと、空気導入管61dの他端側に配置されたコック61eとを有している。導管62は、ビュレット部61と測定台63との間に取り付けられている。導管62の内径は6mmである。測定台63の中央部には、直径2mmの穴があいており、導管62が連結されている。測定部64は、円筒64a(アクリル樹脂製)と、円筒64aの底部に接着されたナイロンメッシュ64bと、重り64cとを有している。円筒64aの内径は20mmである。ナイロンメッシュ64bの目開きは75μm(200メッシュ)である。そして、測定時にはナイロンメッシュ64b上に測定対象の吸水性樹脂粒子66が均一に撒布される。重り64cの直径は19mmであり、重り64cの質量は119.6gである。重り64cは、吸水性樹脂粒子66上に置かれ、吸水性樹脂粒子66に対して4.14kPaの荷重を加えることができる。
荷重下の吸水量[mL/g]=(Vb-Va)/0.1
(膨潤ゲルの作製)
内容積1000mLのビーカーにイオン交換水398gを量り取った。次に、マグネチックスターラーバー(8mmφ×30mm、リング無し)を用いて1000rpmでイオン交換水を撹拌させながら、ママコができないように吸水性樹脂粒子2.0gをイオン交換水(室温(25℃±2℃))に分散させた。撹拌を続けながら30分間放置し、吸水性樹脂粒子を充分に膨潤させて膨潤ゲルを得た。
ゲルフローレート[g/min]=ゲルフロー量[g]/3[min]
気流型混合装置(有限会社オーテック社製、パッドフォーマー)を用いて、吸水性樹脂粒子10g及び粉砕パルプ6.8gを空気抄造によって均一混合することにより、40cm×12cmの大きさのシート状の吸収体を作製した。次に、シート状の吸収体と同じ大きさを有する坪量16g/m2の2枚のティッシュッペーパーで吸収体の上下を挟んだ状態で全体に196kPaの荷重を30秒間加えてプレスすることにより積層体を得た。さらに、吸収体と同じ大きさを有する坪量22g/m2のポリエチレン-ポリプロピレン製のエアスルー型多孔質液体透過性シートを積層体の上面に配置することにより吸収性物品を作製した。
温度25±2℃の室内において、水平の台の上に吸収性物品を配置した。次に、内径3cmの投入口を有する容量100mLの液投入用シリンダー(両端が開口した円筒)を吸収性物品の主面の中心部に置いた。続いて、あらかじめ少量の青色1号で着色して25±1℃に調整した生理食塩水80mLをシリンダー内に一度に投入した(鉛直方向から供給した)。ストップウォッチを用いて、投入開始から、生理食塩水がシリンダー内から完全に消失するまでの吸収時間を測定した。この操作を30分間隔で更に2回(計3回)行い、3回目の吸収時間を浸透速度[秒]として得た。浸透速度は短い方が好ましい。結果を表1に示す。
Claims (9)
- 生理食塩水の無加圧下の保水量が40g/g以下であり、
中位粒子径が250~370μmであり、
下記(1)~(3)の手順により測定されるゲルフローレートが45.5~50.6g/minである、吸水性樹脂粒子。
(1)前記吸水性樹脂粒子1質量部及び水199質量部を混合することによりゲルを得る。
(2)ロートにおける直径8mmの円形の下端開口を閉止した状態で前記ロートに前記ゲルを収容する。
(3)前記下端開口を開放して3分経過したときの前記ゲルの単位時間あたりの流出量を前記ゲルフローレートとして測定する。 - 荷重4.14kPa下における生理食塩水の吸水量が10~40mL/gである、請求項1に記載の吸水性樹脂粒子。
- (メタ)アクリル酸及びその塩からなる群より選ばれる少なくとも一種に由来する構造単位を有する、請求項1又は2に記載の吸水性樹脂粒子。
- 請求項1~3のいずれか一項に記載の吸水性樹脂粒子を含有する、吸収体。
- 前記吸水性樹脂粒子の含有量が当該吸収体の全質量を基準として50質量%以上である、請求項4に記載の吸収体。
- 請求項4又は5に記載の吸収体を備える、吸収性物品。
- おむつである、請求項6に記載の吸収性物品。
- 下記(1)~(3)の手順により測定されるゲルフローレートに基づき吸水性樹脂粒子を選定する工程を備え、
前記ゲルフローレートが45.5~50.6g/minである、吸水性樹脂粒子の製造方法。
(1)前記吸水性樹脂粒子1質量部及び水199質量部を混合することによりゲルを得る。
(2)ロートにおける直径8mmの円形の下端開口を閉止した状態で前記ロートに前記ゲルを収容する。
(3)前記下端開口を開放して3分経過したときの前記ゲルの単位時間あたりの流出量を前記ゲルフローレートとして測定する。 - 吸収体を備える吸収性物品における浸透速度の調整方法であって、
前記吸収体が吸水性樹脂粒子を含有し、
当該調整方法が、下記(1)~(3)の手順により測定されるゲルフローレートを調整する工程を備え、
前記ゲルフローレートが45.5~50.6g/minである、浸透速度の調整方法。
(1)前記吸水性樹脂粒子1質量部及び水199質量部を混合することによりゲルを得る。
(2)ロートにおける直径8mmの円形の下端開口を閉止した状態で前記ロートに前記ゲルを収容する。
(3)前記下端開口を開放して3分経過したときの前記ゲルの単位時間あたりの流出量を前記ゲルフローレートとして測定する。
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