JP7146333B2 - 多孔性高吸水性樹脂の製造方法 - Google Patents
多孔性高吸水性樹脂の製造方法 Download PDFInfo
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Description
本出願は、2016年12月26日付韓国特許出願第10-2016-0179492号に基づいた優先権の利益を主張し、当該韓国特許出願の文献に開示されたすべての内容は本明細書の一部として含まれる。
一方、このような単量体組成物を熱重合または光重合して含水ゲル重合体を形成する方法もまた通常用いられる重合方法であれば、特に構成の限定がない。
[式1]
CRC(g/g)={[W2(g)-W1(g)]/W0(g)}-1
W0(g)は高吸水性樹脂の初期重量(g)であり、W1(g)は高吸水性樹脂を使用せず、遠心分離機を用いて250Gで3分間脱水した後に測定した装置重量であり、W2(g)は常温で0.9重量%の生理食塩水に高吸水性樹脂を30分間浸水して吸収させた後、遠心分離機を用いて250Gで3分間脱水した後に、高吸水性樹脂を含めて測定した装置重量である。
[式2]
AUP(g/g)=[W4(g)-W3(g)]/W0(g)
W0(g)は高吸水性樹脂の初期重量(g)であり、W3(g)は高吸水性樹脂の重量及び前記高吸水性樹脂に荷重を付与できる装置重量の総和であり、W4(g)は荷重(0.7psi)下に1時間前記高吸水性樹脂に生理食塩水を吸収させた後に、高吸水性樹脂の重量及び前記高吸水性樹脂に荷重を付与できる装置重量の総和である。
1)前記高吸水性樹脂に生理食塩水を吸収させて膨潤させる段階;2)前記膨潤された高吸水性樹脂を所定の間隔を有するレオメータのプレートの間に位置させて両プレート面を加圧する段階;3)振動下のレオメータを用いてせん断変形を増加させながら、貯蔵弾性率(storage modulus)と、損失弾性率(loss modulus)が一定の線線状粘弾性状態(linear viscoelastic regime)区間のせん断変形を確認する段階;及び4)前記確認されたせん断変形下で前記膨潤された高吸水性樹脂の貯蔵弾性率と、損失弾性率とをそれぞれ測定し、前記貯蔵弾性率の平均値をゲル強度として測定する段階。
アクリル酸35.83g、苛性ソーダ(NaOH、30重量%溶液)56.54g及び水7.76gを混合して前記アクリル酸の約90モル%が中和した中和液を製造した。
前記Pluronic(登録商標)P123[ポリ(エチレンオキシド)(プロピレンオキシド)(エチレンオキシド)3ブロック共重合体]の代わりにPluronic(登録商標)F127[ポリ(エチレンオキシド)(プロピレンオキシド)(エチレンオキシド)3ブロック共重合体]を用いた点を除いては、実施例1と同様の方法で実施例2の多孔性高吸水性樹脂を製造した。
アクリル酸35.83g、苛性ソーダ(NaOH、30重量%溶液)43.54g及び水7.76gを混合して前記アクリル酸の70モル%が中和した中和液を製造した。
アクリル酸35.83g、苛性ソーダ(NaOH、30重量%溶液)43.54g及び水7.76gを混合して前記アクリル酸の約70モル%が中和した中和液を形成した点を除いては、実施例1と同様の方法で高吸水性樹脂を得た。
前記実施例及び比較例の高吸水性樹脂に対して次のような方法で物性評価を行い、測定された物性値は下記表1に示すとおりである。
ヨーロッパ不織布産業協会(European Disposables and Nonwovens Association、EDANA)の規格であるEDANA WSP 241.2に従い実施例及び比較例の高吸水性樹脂に対して、無荷重下吸収倍率による遠心分離保持能(CRC)を測定した。
CRC(g/g)={[W2(g)-W1(g)]/W0(g)}-1
W0(g)は高吸水性樹脂の初期重量(g)であり、
W1(g)は高吸水性樹脂を使用せず、遠心分離機を用いて250Gで3分間脱水した後に測定した装置重量であり、
W2(g)は常温で0.9重量%生理食塩水に高吸水性樹脂を30分間の浸水して吸収させた後、遠心分離機を用いて250Gで3分間脱水した後に、高吸水性樹脂を含めて測定した装置重量である。
前記実施例及び比較例それぞれで製造された高吸水性樹脂中の300μm~500μmの粒径を有する試料2.0gを分離して100mLのフラスコに入れた後、50mLの0.9重量%塩化ナトリウム水溶液を添加して600rpmで攪拌しながら自由膨潤させた。そして、前記攪拌により発生する液体の渦巻(vortex)が無くなってなめらかな表面ができる時点までの時間を測定した。
Claims (9)
- 酸性基を有する水溶性エチレン系不飽和単量体を80モル%以上中和した中和液に、内部架橋剤、開始剤、無機フィラー及び非イオン性界面活性剤を添加して単量体中和液を形成する段階;
前記単量体中和液を1,000~20,000rpmの速度で混合する段階;
熱重合または光重合により前記高せん断混合された単量体中和液から含水ゲル重合体を形成する段階;及び
前記含水ゲル重合体を乾燥、粉砕及び分級してベース樹脂粉末を形成する段階;を含み、
前記無機フィラーは、(メタ)アクリレート系官能基、アリル基、ビニル基、エポキシ基、ヒドロキシ基、イソシアネート基及びアミン基からなる群より選ばれた少なくとも1種以上の官能基を含む架橋性または親水性官能基に表面改質されたシリカナノ粒子またはアルミナナノ粒子であり、
前記非イオン性界面活性剤は、アルキレングリコール、ポリエチレングリコール、ポリ(エチレン-プロピレン)グリコール、ポリビニルアルコール、ポリオキシエチレンアルキルエーテル、脂肪酸ジエタノールアミン及びアルキルモノグリセリルエーテルからなる群より選ばれた1種以上を含む、多孔性高吸水性樹脂の製造方法。 - 前記非イオン性界面活性剤は、前記酸性基を有する水溶性エチレン系不飽和単量体100重量部に対して0.1~5重量部で使用される、請求項1に記載の多孔性高吸水性樹脂の製造方法。
- 前記単量体中和液を高せん断混合する段階は、1分~100分間行われる、請求項1に記載の多孔性高吸水性樹脂の製造方法。
- 酸性基を有する水溶性エチレン系不飽和単量体に塩基性化合物を添加して80モル%以上中和した中和液を形成する段階をさらに含む、請求項1に記載の多孔性高吸水性樹脂の製造方法。
- 前記水溶性エチレン系不飽和単量体は、アクリル酸、メタクリル酸、無水マレイン酸、フマル酸、クロトン酸、イタコン酸、2-アクリロイルエタンスルホン酸、2-メタクリロイルエタンスルホン酸、2-(メタ)アクリロイルプロパンスルホン酸、または2-(メタ)アクリルアミド-2-メチルプロパンスルホン酸の陰イオン性単量体とその塩;(メタ)アクリルアミド、N-置換(メタ)アクリレート、2-ヒドロキシエチル(メタ)アクリレート、2-ヒドロキシプロピル(メタ)アクリレート、メトキシポリエチレングリコール(メタ)アクリレートまたはポリエチレングリコール(メタ)アクリレートの非イオン系親水性含有単量体;及び(N,N)-ジメチルアミノエチル(メタ)アクリレートまたは(N,N)-ジメチルアミノプロピル(メタ)アクリルアミドのアミノ基含有不飽和単量体とその4級化物;からなる群より選ばれた1種以上を含む、請求項1に記載の多孔性高吸水性樹脂の製造方法。
- 前記内部架橋剤は、ポリエチレングリコールジアクリレート(PEGDA)、グリセリンジアクリレート、グリセリントリアクリレート、非改質またはエトキシル化されたトリメチロールトリアクリレート(TMPTA)、ヘキサンジオールジアクリレート、及びトリエチレングリコールジアクリレートからなる群より選ばれた1種以上を含む、請求項1に記載の多孔性高吸水性樹脂の製造方法。
- 表面架橋剤の存在下で、前記ベース樹脂粉末の表面を追加架橋して表面架橋層を形成する段階をさらに含む、請求項1に記載の多孔性高吸水性樹脂の製造方法。
- 前記表面架橋剤は、エチレングリコール、1,4-ブタンジオール、1,6-ヘキサンジオール、プロピレングリコール、1,2-ヘキサンジオール、1,3-ヘキサンジオール、2-メチル-1,3-プロパンジオール、2,5-ヘキサンジオール、2-メチル-1,3-ペンタンジオール、2-メチル-2,4-ペンタンジオール、トリプロピレングリコール、グリセロール、エチレンカーボネート及びプロピレンカーボネートからなる群より選ばれた1種以上を含む、請求項7に記載の多孔性高吸水性樹脂の製造方法。
- 前記単量体中和液のうちの水溶性エチレン系不飽和単量体の含有量は、20~約60重量%である、請求項1に記載の多孔性高吸水性樹脂の製造方法。
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