JP5901524B2 - 吸水性樹脂 - Google Patents
吸水性樹脂 Download PDFInfo
- Publication number
- JP5901524B2 JP5901524B2 JP2012529560A JP2012529560A JP5901524B2 JP 5901524 B2 JP5901524 B2 JP 5901524B2 JP 2012529560 A JP2012529560 A JP 2012529560A JP 2012529560 A JP2012529560 A JP 2012529560A JP 5901524 B2 JP5901524 B2 JP 5901524B2
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- JP
- Japan
- Prior art keywords
- water
- absorbent resin
- absorbent
- slurry
- primary particles
- 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.)
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Description
本発明にかかる吸水性樹脂は、逆相懸濁重合法によって水溶性エチレン性不飽和単量体を重合して製造される1次粒子を、さらに逆相懸濁重合法によって凝集させて形成される。
本発明にかかる製造方法は2段以上の逆相懸濁重合法によって実施される。より具体的には、下記の工程1及び2を含む製造方法が挙げられる。
(1)分散安定剤の存在下に水溶性エチレン性不飽和単量体を逆相懸濁重合法によって重合し、1次粒子が分散するスラリーを作製する工程1。
(2)工程1にて得られるスラリーに、水溶性エチレン性不飽和単量体を加えて重合反応させる逆相懸濁重合法によって、該スラリー中に分散する1次粒子を凝集させる工程2。
本工程における逆相懸濁重合法とは、分散安定剤を含む分散媒に、水溶性エチレン性不飽和単量体を含む水溶液を添加し、撹拌することで懸濁させ、分散した水溶液中にて水溶性エチレン性不飽和単量体を重合させる方法である。よって、工程1では分散媒中に単量体が重合して製造される上述の中位粒子径の範囲を満たす1次粒子が分散するスラリーが得られる。
工程2では、工程1にて得られる1次粒子が分散するスラリーに、水溶性エチレン性不飽和単量体を含む水溶液を加えて単量体を重合反応させる逆相懸濁重合法によって、該スラリー中に分散する1次粒子を凝集させる。
本発明にかかる吸収体は、上述した吸水性樹脂と親水性繊維より構成されている。吸収体の構成としては、例えば、吸水性樹脂と親水性繊維を均一な組成となるように混合することによって得られた混合分散体、層状の親水性繊維の間に吸水性樹脂が挟まれたサンドイッチ構造体、吸水性樹脂と親水性繊維とをティッシュで包んだ構造体等が挙げられるが、本発明はかかる例示に限定されるものではない。
別に規定のない限り、吸水性樹脂の粒径を中位粒子径として規定し、次のようにして測定した。吸水性樹脂50gに、滑剤として、0.25gの非晶質シリカ(デグサジャパン(株)、Sipernat200)を混合した。
吸水性樹脂約2gを、あらかじめ秤量したアルミホイールケース(8号)に精秤した(Wa(g))。上記サンプルを、内温を105℃に設定した熱風乾燥機(ADVANTEC社製)で2時間乾燥させた後、デシケーター中で放冷して、乾燥後の吸水性樹脂の質量Wb(g)を測定した。以下の式から、吸水性樹脂の水分率を算出した。
水分率(%)=[Wa―Wb]/Wa×100
500mL容のビーカーに、0.9質量%塩化ナトリウム水溶液(生理食塩水)500gを量り取り、600r/minで撹拌させながら、吸水性樹脂2.0gを、ママコが発生しないように分散させた。撹拌させた状態で30分間放置し、吸水性樹脂を十分に膨潤させた。その後、綿袋(メンブロード60番、横100mm×縦200mm)中に注ぎ込み、綿袋の上部を輪ゴムで縛り、遠心力が167Gとなるよう設定した脱水機(国産遠心機株式会社製、品番:H−122)を用いて綿袋を1分間脱水し、脱水後の膨潤ゲルを含んだ綿袋の質量Wc(g)を測定した。吸水性樹脂を添加せずに同様の操作を行ない、綿袋の湿潤時の空質量Wd(g)を測定し、以下の式から保水能を算出した。
生理食塩水保水能(g/g)=[Wc−Wd](g)/吸水性樹脂の質量(g)
本試験は、25℃±1℃に調節された室内で行った。100mL容のビーカーに、生理食塩水50±0.1gを量りとり、マグネチックスターラーバー(8mmφ×30mmのリング無し)を投入し、ビーカーを恒温水槽に浸漬して、液温を25±0.2℃に調節した。次に、マグネチックスターラー上にビーカーを置いて、回転数600r/minとして、生理食塩水に渦を発生させた後、吸水性樹脂2.0±0.002gを、前記ビーカーに素早く添加し、ストップウォッチを用いて、吸水性樹脂の添加後から液面の渦が収束する時点までの時間(秒)を測定し、吸水性樹脂の吸水速度とした。
(a)合成尿の調整
1L容の容器に、塩化カリウム2g、無水硫酸ナトリウム2g、塩化カルシウム0.19g、塩化マグネシウム0.23g、リン酸二水素アンモニウム0.85g、リン酸一水素アンモニウム0.15g及び適量の蒸留水を入れ、完全に溶解した。更に蒸留水を追加して、水溶液全体の体積を1Lに調整した。
測定装置として、図1に機略構成を示したものを用いた。装置としては、タンク11には、静圧調整用ガラス管12が具備されており、ガラス管12の下端は、0.69質量%塩化ナトリウム水溶液13のシリンダー22内の液面の高さが膨潤ゲル25の底部から、5cm上の高さに維持できるように配置した。タンク11中の0.69質量%塩化ナトリウム水溶液13は、コック付L字管14を通じてシリンダー22内へ供給された。シリンダー22の下には、通過した液を捕集する容器33を配置し、捕集容器33を上皿天秤34の上に配置した。シリンダー22の内径は6cmであり、下部の底面にはNo.400ステンレス製金網(目開き38μm)26が設置されていた。ピストン型重り21の下部には液が通過するのに十分な穴23があり、底部には吸水性樹脂あるいはそれらの膨潤ゲルが、穴23へ入り込まないように透過性の良いガラスフィルター24が取り付けた。
円筒状容器20に0.9gの吸水性樹脂を均一に入れ、吸水性樹脂を合成尿中で、ピストン型重り21を用いて2.07kPaの荷重下で60分間膨潤させ、膨潤ゲル25を形成した。
還流冷却器、滴下ロート、窒素ガス導入管並びに攪拌機として、翼径50mmの4枚傾斜パドル翼を2段で有する撹拌翼を備えた内径110mm、2L容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n−ヘプタン340gをとり、HLB3のショ糖ステアリン酸エステル(三菱化学フーズ(株)、リョートーシュガーエステルS−370)0.92g、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)、ハイワックス1105A)0.92gを添加し、撹拌しつつ80℃まで昇温して界面活性剤を溶解した後、50℃まで冷却した。
実施例1において、第1段目の攪拌機の回転数を300r/minに変更した以外は、実施例1と同様の操作を行い、球状粒子が凝集した形態の吸水性樹脂(B)233.5gを得た。1次粒子の中位粒子径は130μm、吸水性樹脂の中位粒子径は415μm、水分率は7.3%であった。各性能の測定結果を表1に示す。
実施例2において、第2段目重合後のn−ヘプタン還流による脱水量を217gに変更した以外は、実施例2と同様の操作を行い、球状粒子が凝集した形態の吸水性樹脂(C)232.9gを得た。1次粒子の中位粒子径は130μm、吸水性樹脂の中位粒子径は424μm、水分率は10.0%であった。各性能の測定結果を表1に示す。
還流冷却器、滴下ロート、窒素ガス導入管並びに攪拌機として、翼径50mmの4枚傾斜パドル翼を2段で有する撹拌翼を備えた内径110mm、2L容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n−ヘプタン340gをとり、HLB3のショ糖ステアリン酸エステル(三菱化学フーズ(株)、リョートーシュガーエステルS−370)0.92g、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)、ハイワックス1105A)0.92gを添加し、撹拌しつつ80℃まで昇温して界面活性剤を溶解した後、50℃まで冷却した。
実施例4において、第1段目の攪拌機の回転数を500r/minに変更し、第2段目重合後のn−ヘプタン還流による脱水量を213gに変更した以外は、実施例4と同様の操作を行い、球状粒子が凝集した形態の吸水性樹脂(E)232.8gを得た。1次粒子の中位粒子径は230μm、吸水性樹脂の中位粒子径は458μm、水分率は10.0%であった。各性能の測定結果を表1に示す。
実施例5において、第1段目の攪拌機の回転数を400r/minに変更した以外は、実施例5と同様の操作を行い、球状粒子が凝集した形態の吸水性樹脂(F)234.2gを得た。1次粒子の中位粒子径は250μm、吸水性樹脂の中位粒子径は470μm、水分率は7.2%であった。各性能の測定結果を表1に示す。
実施例1において、第1段目の攪拌機の回転数を500r/minに変更し、第2段目重合後のn−ヘプタン還流による脱水量を230gに変更した以外は、実施例1と同様の操作を行い、球状粒子が凝集した形態の吸水性樹脂(G)229.6gを得た。1次粒子の中位粒子径は90μm、吸水性樹脂の中位粒子径は364μm、水分率は7.0%であった。各性能の測定結果を表1に示す。
実施例4において、第1段目の攪拌機の回転数を350r/minに変更し、第2段目重合後のn−ヘプタン還流による脱水量を213gに変更した以外は、実施例4と同様の操作を行い、球状粒子が凝集した形態の吸水性樹脂(H)227.6gを得た。1次粒子の中位粒子径は280μm、吸水性樹脂の中位粒子径は519μm、水分率は6.9%であった。各性能の測定結果を表1に示す。
実施例2において、第2段目重合後のn−ヘプタン還流による脱水量を230gに変更した以外は、実施例2と同様の操作を行い、球状粒子が凝集した形態の吸水性樹脂(I)231.7gを得た。1次粒子の中位粒子径は130μm、吸水性樹脂の中位粒子径は420μm、水分率は6.4%であった。各性能の測定結果を表1に示す。
実施例5において、第2段目重合後のn−ヘプタン還流による脱水量を233gに変更した以外は、実施例5と同様の操作を行い、球状粒子が凝集した形態の吸水性樹脂(J)233.4gを得た。1次粒子の中位粒子径は230μm、吸水性樹脂の中位粒子径は448μm、水分率は5.4%であった。各性能の測定結果を表1に示す。
実施例1で得られた吸水性樹脂(A)10gと粉砕パルプ10gをミキサーを用いて乾式混合したものを、大きさが40cm×12cmで重さが1gのティッシュに吹き付けた後に、同じ大きさ及び重さのティッシュを上部から重ねてシート状にし、これの全体に196kPaの荷重を30秒間加えてプレスすることにより、吸収体を得た。得られた吸収体を大きさ40cm×12cm、坪量20g/m2のポリエチレン製エアスルー型多孔質液体透過性シートと、同じ大きさ、同じ坪量のポリエチレン製不透過性シートで挟みつけることにより吸収体を用いた吸収性物品を得た。
実施例7において、実施例2で得られた吸水性樹脂(B)を用いた以外は、実施例7と同様にして、吸収体及びそれを用いた吸収性物品を得た。
実施例7において、実施例3で得られた吸水性樹脂(C)を用いた以外は、実施例7と同様にして、吸収体及びそれを用いた吸収性物品を得た。
実施例7において、実施例4で得られた吸水性樹脂(D)を用いた以外は、実施例7と同様にして、吸収体及びそれを用いた吸収性物品を得た。
実施例7において、実施例5で得られた吸水性樹脂(E)を用いた以外は、実施例7と同様にして、吸収体及びそれを用いた吸収性物品を得た。
実施例7において、実施例6で得られた吸水性樹脂(F)を用いた以外は、実施例7と同様にして、吸収体及びそれを用いた吸収性物品を得た。
実施例7において、比較例1で得られた吸水性樹脂(G)を用いた以外は、実施例7と同様にして、吸収体及びそれを用いた吸収性物品を得た。
実施例7において、比較例2で得られた吸水性樹脂(H)を用いた以外は、実施例7と同様にして、吸収体及びそれを用いた吸収性物品を得た。
実施例7において、比較例3で得られた吸水性樹脂(I)を用いた以外は、実施例7と同様にして、吸収体及びそれを用いた吸収性物品を得た。
実施例7において、比較例4で得られた吸水性樹脂(J)を用いた以外は、実施例7と同様にして、吸収体及びそれを用いた吸収性物品を得た。
(a)人工尿の調整
10L容の容器に、塩化ナトリウム60g、塩化カルシウム二水和物1.8g、塩化マグネシウム六水和物3.6g及び適量の蒸留水を入れ、完全に溶解させた。次に、1質量%ポリ(オキシエチレン)イソオクチルフェニルエーテル水溶液15gを添加し、さらに蒸留水を添加して、水溶液全体の質量を6000gに調整した後、少量の青色1号で着色して、人工尿を調製した。
(b)浸透速度
吸収性物品の中心付近に、内径3cmの円筒型シリンダーを置き、50mLの人工尿をそのシリンダー内に一度に投入するとともに、ストップウォッチを用いて、人工尿がシリンダー内から完全に消失するまでの時間を測定し、1回目の浸透速度(秒)とした。次に、前記シリンダーをはずし、吸収性物品をそのままの状態で保存し、1回目の人工尿投入開始から30分後及び60分後にも、1回目と同じ位置に前記円筒型シリンダーを置いて同様の操作を行い、2回目及び3回目の浸透速度(秒)を測定した。1回目〜3回目の秒数の合計を合計浸透速度とした。
(c)逆戻り量
前記浸透速度の測定終了から60分経過後、吸収性物品上の人口尿投入位置付近に、あらかじめ質量(We(g)、約70g)を測定しておいた10cm四方の濾紙(約80枚)を置き、その上に底面が10cm×10cmの5kgの重りを載せた。5分間の荷重後、濾紙の質量(Wf(g))を測定し、増加した質量を逆戻り量(g)とした。
液体逆戻り量(g)=Wf−We
(d)拡散長
前記逆戻り量の測定後5分以内に、人口尿が浸透したそれぞれの吸収性物品の長手方向の拡がり寸法(cm)を測定した。なお、小数点以下の数値は四捨五入した。
12 静圧調整用ガラス管
13 0.69質量%塩化ナトリウム水溶液
14 コック付L字管
15 コック
20 円筒状容器
21 ピストン型重り
22 シリンダー
23 穴
24 ガラスフィルター
25 膨潤ゲル
26 ステンレス金網
31 漏斗
32 支持台
33 捕集容器
34 上皿天秤
Claims (7)
- 吸水性樹脂の製造方法であって、
(1)分散安定剤の存在下に水溶性エチレン性不飽和単量体を逆相懸濁重合法によって重合し、中位粒子径が100〜250μmである1次粒子が分散するスラリーを作製する工程、及び
(2)工程(1)にて得られるスラリーに、水溶性エチレン性不飽和単量体を加えて重合反応させる逆相懸濁重合法によって、該スラリー中に分散する1次粒子を凝集させて、生理食塩水保水能が30g/g以下である吸水性樹脂を製造する工程、
を含む製造方法。 - 吸水性樹脂の0.69質量%塩化ナトリウム水溶液の通液速度が、200g/10分以上である、請求項1に記載の吸水性樹脂の製造方法。
- 吸水性樹脂の生理食塩水吸水速度が、45秒以上180秒以下である、請求項1又は2に記載の吸水性樹脂の製造方法。
- 分散安定剤が、ショ糖脂肪酸エステル及びポリグリセリン脂肪酸エステルからなる群より選ばれた少なくとも1種である請求項1〜3のいずれか1項に記載の吸水性樹脂の製造方法。
- 水溶性エチレン性不飽和単量体が、(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1つである請求項1〜4のいずれか1項に記載の吸水性樹脂の製造方法。
- 吸収体の製造方法であって、
(1)分散安定剤の存在下に水溶性エチレン性不飽和単量体を逆相懸濁重合法によって重合し、中位粒子径が100〜250μmである1次粒子が分散するスラリーを作製する工程、
(2)工程(1)にて得られるスラリーに、水溶性エチレン性不飽和単量体を加えて重合反応させる逆相懸濁重合法によって、該スラリー中に分散する1次粒子を凝集させて、生理食塩水保水能が30g/g以下である吸水性樹脂を製造する工程、及び
(3)工程(2)にて得られる吸水性樹脂、及び親水性繊維から吸収体を製造する工程、
を含む製造方法。 - 吸収性物品の製造方法であって、
(1)分散安定剤の存在下に水溶性エチレン性不飽和単量体を逆相懸濁重合法によって重合し、中位粒子径が100〜250μmである1次粒子が分散するスラリーを作製する工程、
(2)工程(1)にて得られるスラリーに、水溶性エチレン性不飽和単量体を加えて重合反応させる逆相懸濁重合法によって、該スラリー中に分散する1次粒子を凝集させて、生理食塩水保水能が30g/g以下である吸水性樹脂を製造する工程、
(3)工程(2)にて得られる吸水性樹脂、及び親水性繊維から吸収体を製造する工程、及び
(4)工程(3)にて得られる吸収体を、液体透過性シートと液体不透過性シートとの間に保持する工程、
を含む製造方法。
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WO2012023433A1 (ja) | 2012-02-23 |
BR112013003873A2 (pt) | 2016-07-05 |
KR20130099050A (ko) | 2013-09-05 |
TW201223970A (en) | 2012-06-16 |
EP2607383B1 (en) | 2018-12-19 |
CN103080140A (zh) | 2013-05-01 |
BR112013003873B1 (pt) | 2020-01-28 |
EP2607383A4 (en) | 2014-11-05 |
SA111320691B1 (ar) | 2014-08-25 |
US20130130017A1 (en) | 2013-05-23 |
EP2607383A1 (en) | 2013-06-26 |
CN103080140B (zh) | 2014-11-19 |
KR101760768B1 (ko) | 2017-07-24 |
SG187061A1 (en) | 2013-02-28 |
JPWO2012023433A1 (ja) | 2013-10-28 |
TWI501979B (zh) | 2015-10-01 |
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