JP2009519356A - 熱可塑性物質で被覆された高吸収性ポリマー組成物 - Google Patents
熱可塑性物質で被覆された高吸収性ポリマー組成物 Download PDFInfo
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- JP2009519356A JP2009519356A JP2008544674A JP2008544674A JP2009519356A JP 2009519356 A JP2009519356 A JP 2009519356A JP 2008544674 A JP2008544674 A JP 2008544674A JP 2008544674 A JP2008544674 A JP 2008544674A JP 2009519356 A JP2009519356 A JP 2009519356A
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- superabsorbent polymer
- polymer composition
- superabsorbent
- gel bed
- bed permeability
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Abstract
Description
自由膨張ゲルベッド浸透性試験
ここで使用されたように、自由膨張ゲルベッド浸透性(GBP)試験は、一般に「自由膨張」と呼ばれる条件下で、ゲル粒子(例えば、表面処理された吸収性材料又は表面処理される前の高吸収性材料)の膨張したベッドの浸透性を決定する。用語「自由膨張」は、後述される試験溶液の吸収において膨張を抑制する荷重を掛けずにゲル粒子を膨張させることを意味する。用語「自由膨張」は、後述される試験溶液の吸収において膨張を抑制する荷重を掛けずに高吸収性ポリマーを膨張させることを意味する。浸透性試験を行うための適切な装置を図1及び図2に示し、全体に28を付した。試験装置28は、全体に30を付したサンプル容器、及び全体に36を付したピストンを含む。ピストン36は、シャフトの長軸に沿って開けられた同心円筒孔40を有する円筒状LEXAN(登録商標)シャフト38を含む。シャフト38の両端は機械加工され、各々42、46を付した上端及び下端を提供する。48を付した重りは、一方の端42の上に載っていて、その中心の少なくとも一部を通して開けた円筒孔48aを有する。
ここで用いたように、負荷ゲルベッド浸透性(GBP)試験(或いはここでは0.3psiでのGBPという)によって、一般に「荷重を受けた(負荷)」条件下と呼ばれる条件下で、ゲル粒子(例えば、それらの用語として高吸収性材料又は吸収性材料がここで使用される)の膨張したベッドの浸透性が決まる。用語「負荷」は、着用者による着座、歩行、ひねり等のように、粒子に適用される通常の使用法の荷重と大抵は一致する荷重によって、粒子の膨張が制限されることを意味する。
遠心分離保持容量(CRC)試験は、高吸収性ポリマーが飽和し、管理条件下で遠心分離を受けた後に、その中に液体を保持する能力を測定する。得られた保持容量は、保持された液体のグラム/サンプルのグラム質量(g/g)として示される。試験用サンプルは、米国規格の30メッシュスクリーンにより事前に篩い分けし、米国規格の50メッシュスクリーン上に残した粒子から調製する。結果として、高吸収性ポリマーサンプルは、約300〜600μmの範囲の寸法の粒子を含む。粒子は、手動で又は自動で事前に篩い分けできる。
オーブンシェイクアウト試験は、高吸収性ポリマー自体をポリオレフィン材料と親和させる高吸収性ポリマーの能力を測定する。オーブンシェイクアウト試験は、ポリオレフィンからのSAPシェイクアウト(%)又は高吸収性組成物シェイクアウトとして表される。この試験に必要な材料としては、4インチ(inch)直径のアルミニウム秤量皿、ポリエチレンZIPLOC(登録商標)袋、高吸収性ポリマー粒子(SAP)、0.5インチのアルミニウムプレート、従来型の空気オーブン、Retsch Vibro篩い分け機(品番30.403.009)、底皿及び12〜20メッシュスクリーンが挙げられる。
断熱した平底の反応容器内で、1866.7gの50%NaOHを3090.26gの蒸留水に加え、25℃に冷却した。次に800gのアクリル酸を水酸化ナトリウム溶液に加え、その溶液を再び25℃に冷却した。次に、終始撹拌しながら、アクリル酸中に50質量%メトキシポリエチレングリコールモノメタクリレート120gを含む1600gのアクリル酸及び14.4gのエトキシ化トリメチロールプロパントリアクリレートの第二の溶液を第一の溶液に加え、続いて15℃に冷却し、10molをエトキシル化した14.4gのヒドロキシモノアリルエーテルを加え、さらに5℃に冷却した。次に、断熱条件下で、100ppmの過酸化水素、200ppmのアゾ‐ビス‐(2‐アミジノ‐プロペン)二塩酸塩、200ppmの過硫酸ナトリウム及び40ppmのアスコルビン酸(全て水溶液)の混合物を用いてモノマー溶液を重合させ、最大温度(Tmax)付近で25分間続けた。得られたゲルを切り刻み、Hobart 4M6工業用押出し機を用いて押し出し、次に最終製品の水分濃度が5質量%未満になるまでProcter & Schwartz 062型熱風オーブン内で、20インチ×40インチの孔あき金属トレイ上で、上昇風10分間及び下降風6分間、175℃で乾燥した。乾燥した材料は、Prodeva 315-S型粉砕機内で粗粉砕し、MPI 666-F三段ロールミル内で粉砕し、Minox MTS 600DS3Vを用いて篩い分けして850μmを超える及び150μm未満の粒子を除去した。
比較例1及び実施例2〜4のために表1に従って、3,000gの実施例1の半製品を外界条件で表1に示した量のマレイン酸変性ポリプロピレン25%乳濁液と混合した。具体的には、実施例1の半製品を流動させた。表1に示した量に従って、エチレンカーボネート、熱可塑性塗料及び水を含む吹付液を調製した。吹付液を流動状態の半製品の上に吹き付けた。加えられた水だけでなくMPP乳濁液の寄与を含めて水分量を計算し、吹付混合物を配合して1%のEC、0.0625%のMPP、及び4%の水を得た。次に、吹き付け済みの半製品に24.0gのヒュームドシリカを加えた。全混合物を約1分間流動させた。エチレンカーボネート/熱可塑性物質/水で被覆された半製品を連続パドル乾燥器の中へ、その反応器内の2.5〜3kgの定常状態のポリマー物質を用いて、60〜70g/分で50分間供給した。反応器の後段の途中付近では吸収剤のピーク温度に達したので、この温度を190〜195℃に保った。パドルは25rpmに保った。次に組成物をPEG8000の水溶液でさらに処理した。
実施例4及び実施例5の表3に従って、3,000gの実施例1の半製品を外界条件でマレイン酸変性ポリプロピレン及びエチレンアクリル酸コポリマーの混合物の25%量の水性乳濁液と混合した。具体的には、実施例1の半製品を流動させた。表3に示した量に従って、エチレンカーボネートを温水に溶解させ、マレイン酸変性ポリプロピレンをその溶液に加え、次にエチレンアクリル酸コポリマーをその溶液に加えることにより吹付液を調製した。吹付液を流動状態の半製品の上に吹き付けた。次に、吹き付け済みの半製品に24.0gのヒュームドシリカを加えた。全混合物を約1分間流動させた。エチレンカーボネート/熱可塑性物質/水で被覆された半製品を連続パドル乾燥器の中へ、その反応器内の2.5〜3kgの定常状態のポリマー物質を用いて、60〜70g/分で50分間供給した。反応器の後段の途中付近で吸収剤のピーク温度に達したので、この温度を190〜195℃に保った。パドルは25rpmに保った。
30 サンプル容器
34 円筒
36 ピストン
38 シャフト
40 同心円筒孔
42 シャフトの上端
46 シャフトの下端
47 環状段部
48 重り
48a 重りの円筒孔
50 円形ピストンヘッド
54 孔
60 孔
62 円筒状の孔
64 ステンレススクリーン
66 ステンレススクリーン
68 サンプル
Claims (54)
- a)高吸収性ポリマーを基準として約55〜99.9質量%の、重合可能な不飽和酸基含有モノマーの高吸収性ポリマー、及び
b)重合可能な不飽和酸基含有モノマーを基準として約0.001〜5質量%の内部架橋剤を含む高吸収性ポリマー
を含む高吸収性ポリマー組成物であって、
前記高吸収性ポリマーは約25%を超える中和度を有し、成分a)及びb)は、さらに
i)乾燥高吸収性ポリマー組成物を基準として約0.001〜5質量%の表面架橋剤、
ii)乾燥高吸収性ポリマー組成物を基準として約0.01〜10質量%の浸透改質剤、
iii)乾燥高吸収性ポリマー組成物を基準として0〜約5質量%の多価金属塩、
iv)乾燥高吸収性ポリマー組成物を基準として0〜約2質量%の界面活性剤、
v)乾燥高吸収性ポリマー組成物を基準として約0.01〜5質量%の不溶性の無機粉末、及び
vi)乾燥高吸収性ポリマー組成物を基準として約0.01〜5質量%の熱可塑性ポリマー
の表面添加剤を含む高吸収性ポリマー粒子状に重合及び調製されて表面処理された高吸収性ポリマー粒子を形成し、
前記表面処理された高吸収性ポリマー粒子が熱処理され、並びに前記高吸収性ポリマー組成物が、遠心分離保持容量試験により測定したときに少なくとも約23g/gの遠心分離保持容量、自由膨張ゲルベッド浸透性試験により測定したときに少なくとも100Darcyの自由膨張ゲルベッド浸透性、及びオーブンシェイクアウト法により測定したときに約20%未満の高吸収性組成物シェイクアウトを示すことを特徴とする高吸収性ポリマー組成物。 - 少なくとも約130Darcyの自由膨張ゲルベッド浸透性を有する請求項1に記載の高吸収性ポリマー組成物。
- 少なくとも約160Darcyの自由膨張ゲルベッド浸透性を有する請求項1に記載の高吸収性ポリマー組成物。
- 少なくとも約200Darcyの自由膨張ゲルベッド浸透性を有する請求項1に記載の高吸収性ポリマー組成物。
- 高吸収性組成物シェイクアウトが約16%未満である請求項1に記載の高吸収性ポリマー組成物。
- 乾燥高吸収性ポリマー組成物を基準として約0.1〜5質量%の多価金属塩を含む請求項1に記載の高吸収性ポリマー組成物。
- 熱可塑性ポリマーが、ポリオレフィン、ポリエチレン、ポリエステル、ポリウレタン、線状低密度ポリエチレン(LLDPE)、エチレンアクリル酸コポリマー(EAA)、スチレンコポリマー、エチレンメタクリル酸アルキルコポリマー(EMA)、ポリプロピレン(PP)、マレイン酸変性ポリプロピレン(MPP)、エチレン酢酸ビニルコポリマー(EVA)、ポリアミド、ポリエステル、並びにこれらの混合物及びコポリマーからなる群から選択される請求項1に記載の高吸収性ポリマー組成物。
- 高吸収性ポリマー粒子がカチオン性ポリマーで被覆されている請求項1に記載の高吸収性ポリマー組成物。
- カチオン性ポリマーがポリビニルアミンである請求項8に記載の高吸収性ポリマー組成物。
- 負荷ゲルベッド浸透性試験により測定したときに少なくとも約4Darcyの負荷ゲルベッド浸透性を有する請求項1に記載の高吸収性ポリマー組成物。
- 負荷ゲルベッド浸透性試験により測定したときに少なくとも約8Darcyの負荷ゲルベッド浸透性を有する請求項1に記載の高吸収性ポリマー組成物。
- 負荷ゲルベッド浸透性試験により測定したときに少なくとも約10Darcyの負荷ゲルベッド浸透性を有する請求項1に記載の高吸収性ポリマー組成物。
- 少なくとも約25g/gの遠心分離保持容量を有する請求項1に記載の高吸収性ポリマー組成物。
- 熱可塑性ポリマーがマレイン酸変性ポリプロピレンである請求項1に記載の高吸収性ポリマー組成物。
- 熱可塑性ポリマーが、マレイン酸変性ポリプロピレン及びエチレンアクリル酸コポリマーの混合物である請求項1に記載の高吸収性ポリマー組成物。
- 不溶性の無機粉末がシリカである請求項1に記載の高吸収性ポリマー組成物。
- 表面架橋剤で表面処理された及び熱可塑性の、わずかに架橋したポリマーを含み、オーブンシェイクアウト法による約20%未満の高吸収性組成物シェイクアウトを有する高吸収性ポリマー組成物。
- 少なくとも約100Darcyの自由膨張ゲルベッド浸透性を有する請求項17に記載の高吸収性ポリマー組成物。
- 少なくとも約130Darcyの自由膨張ゲルベッド浸透性を有する請求項17に記載の高吸収性ポリマー組成物。
- 少なくとも約160Darcyの自由膨張ゲルベッド浸透性を有する請求項17に記載の高吸収性ポリマー組成物。
- 少なくとも約200Darcyの自由膨張ゲルベッド浸透性を有する請求項17に記載の高吸収性ポリマー組成物。
- 少なくとも約4Darcyの負荷自由膨張ゲルベッド浸透性を有する請求項17に記載の高吸収性ポリマー組成物。
- 少なくとも約8Darcyの負荷自由膨張ゲルベッド浸透性を有する請求項17に記載の高吸収性ポリマー組成物。
- 少なくとも約23g/gの遠心分離保持容量を有する請求項17に記載の高吸収性ポリマー組成物。
- 少なくとも約25g/gの遠心分離保持容量を有する請求項17に記載の高吸収性ポリマー組成物。
- 約16%未満の高吸収性組成物シェイクアウトを有する請求項17に記載の高吸収性ポリマー組成物。
- 熱可塑性ポリマーがマレイン酸変性ポリプロピレンの混合物である請求項17に記載の高吸収性ポリマー組成物。
- 熱可塑性ポリマーがマレイン酸変性ポリプロピレン及びエチレンアクリル酸コポリマーの混合物である請求項17に記載の高吸収性ポリマー組成物。
- a)高吸収性ポリマーを基準として約55〜99.9質量%の重合可能な不飽和酸基含有モノマー、及び前記重合可能な不飽和酸基含有モノマーを基準として約0.001〜5質量%の内部架橋剤を重合する方法により、約25%を超える中和度を有する高吸収性ポリマーを調製する工程、
b)高吸収性ポリマーから高吸収性ポリマー粒子を調製する工程、
c)i)乾燥高吸収性ポリマー組成物を基準として約0.001〜5質量%の表面架橋剤、
ii)乾燥高吸収性ポリマー組成物を基準として約0.01〜10質量%の浸透改質剤、
iii)乾燥高吸収性ポリマー組成物を基準として0〜約5質量%の多価金属塩、
iv)乾燥高吸収性ポリマー組成物を基準として0〜約2質量%の界面活性剤、
v)乾燥高吸収性ポリマー組成物を基準として約0.01〜5質量%の不溶性の無機粉末、及び
vi)粒子表面上に適用される、乾燥高吸収性ポリマー組成物を基準として約0.01〜5質量%の熱可塑性ポリマーを含む表面添加剤で高吸収性ポリマー粒子を処理する工程、及び
d)被覆された高吸収性ポリマー粒子を熱処理する工程、
を含む高吸収性ポリマー組成物の製造方法であって、
高吸収性ポリマー組成物が、遠心分離保持容量試験により測定したときに少なくとも約23g/gの遠心分離保持容量、自由膨張ゲルベッド浸透性試験により測定したときに少なくとも約100Darcyの自由膨張ゲルベッド浸透性、及びオーブンシェイクアウト法により測定したときに約20%未満の高吸収性組成物シェイクアウトの特性を有することを特徴とする製造方法。 - 工程a)において、酸基の少なくとも約50質量%がカルボキシル基を含み、酸基が少なくとも59mol%中和され、及び内部架橋剤が重合可能な不飽和酸基含有モノマー全量を基準として約1.0〜3.0質量%である請求項29に記載の方法。
- 被覆された高吸収性ポリマーの熱処理が約100〜300℃で行われる請求項29に記載の方法。
- 被覆された高吸収性ポリマーの熱処理が約150〜250℃で行われる請求項29に記載の方法。
- 高吸収性ポリマー組成物が少なくとも約130Darcyの自由膨張ゲルベッド浸透性を有する請求項29に記載の方法。
- 高吸収性ポリマー組成物が少なくとも約160Darcyの自由膨張ゲルベッド浸透性を有する請求項29に記載の方法。
- 高吸収性ポリマー組成物が少なくとも約200Darcyの自由膨張ゲルベッド浸透性を有する請求項29に記載の方法。
- 高吸収性ポリマー組成物が約12%未満の高吸収性組成物シェイクアウトを有する請求項29に記載の方法。
- 高吸収性ポリマー組成物が少なくとも約25g/gの遠心分離保持容量を有す請求項29に記載の方法。
- 熱可塑性ポリマーが、ポリオレフィン、ポリエチレン、ポリエステル、ポリウレタン、線状低密度ポリエチレン(LLDPE)、エチレンアクリル酸コポリマー(EAA)、スチレンコポリマー、エチレンメタクリル酸アルキルコポリマー(EMA)、ポリプロピレン(PP)、マレイン酸変性ポリプロピレン、エチレン酢酸ビニルコポリマー(EVA)、ポリアミド、ポリエステル、並びにこれらの混合物及びコポリマーからなる群から選択される請求項29に記載の方法。
- 高吸収性ポリマー組成物が少なくとも約4Darcyの負荷ゲルベッド浸透性を有する請求項29に記載の方法。
- 高吸収性ポリマー組成物が少なくとも約8Darcyの負荷ゲルベッド浸透性を有する請求項29に記載の方法。
- 高吸収性ポリマー組成物が少なくとも約10Darcyの負荷ゲルベッド浸透性を有する請求項29に記載の方法。
- 熱可塑性ポリマーがマレイン酸変性ポリプロピレンである請求項29に記載の方法。
- 熱可塑性ポリマーがマレイン酸変性ポリプロピレン及びエチレンアクリル酸コポリマーの混合物である請求項29に記載の方法。
- 不溶性の無機粉末がシリカである請求項29に記載の方法。
- さらに表面添加剤がカチオン性ポリマーを含む請求項29に記載の方法。
- カチオン性ポリマーがポリビニルアミンである請求項45に記載の方法。
- 不溶性の無機粉末が不溶性リン酸塩である請求項1に記載の高吸収性ポリマー組成物。
- 不溶性の無機粉末がリン酸アルミニウムである請求項1に記載の高吸収性ポリマー組成物。
- 熱可塑性ポリマーがマレイン酸変性ポリプロピレンであり、不溶性の無機粉末がリン酸アルミニウムである請求項1に記載の高吸収性ポリマー組成物。
- カチオン性ポリマーがポリビニルアミンであり、不溶性の無機粉末がリン酸アルミニウムである請求項8に記載の高吸収性ポリマー組成物。
- 不溶性の無機粉末が不溶性リン酸塩である請求項29に記載の方法。
- 不溶性の無機粉末がリン酸アルミニウムである請求項29に記載の方法。
- 熱可塑性ポリマーがマレイン酸変性ポリプロピレンであり、及び不溶性の無機粉末がリン酸アルミニウムである請求項29に記載の方法。
- カチオン性ポリマーがポリビニルアミンであり、不溶性の無機粉末がリン酸アルミニウムである請求項45に記載の方法。
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- 2007-10-02 US US11/866,054 patent/US7906585B2/en not_active Expired - Fee Related
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2013
- 2013-12-06 JP JP2013253081A patent/JP2014080617A/ja not_active Withdrawn
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JPH06248187A (ja) * | 1993-02-24 | 1994-09-06 | Sanyo Chem Ind Ltd | 吸水剤 |
Cited By (13)
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JP2010510045A (ja) * | 2006-11-10 | 2010-04-02 | ビーエーエスエフ ソシエタス・ヨーロピア | 優れた透過性及び輸送特性を有する超吸収剤 |
JP2012509377A (ja) * | 2008-11-21 | 2012-04-19 | ビーエーエスエフ ソシエタス・ヨーロピア | モノマー溶液の液滴を重合させることによって浸透性の吸水性ポリマー粒子を製造する方法 |
JP2013521962A (ja) * | 2010-03-24 | 2013-06-13 | ビーエーエスエフ ソシエタス・ヨーロピア | 超薄型流体吸収性コア |
JP2013537465A (ja) * | 2010-08-23 | 2013-10-03 | ビーエーエスエフ ソシエタス・ヨーロピア | 超薄流体吸収性コア |
JP2014032126A (ja) * | 2012-08-03 | 2014-02-20 | Central Research Institute Of Electric Power Industry | コンクリートの吸水試験装置、並びに、コンクリートの透過係数分布の推定方法、推定装置及び推定プログラム |
JPWO2015178481A1 (ja) * | 2014-05-23 | 2017-05-25 | Sdpグローバル株式会社 | 吸水性樹脂粒子、これを含む吸収体および吸収性物品 |
US10174174B2 (en) | 2014-05-23 | 2019-01-08 | Sdp Global Co., Ltd. | Water-absorbing resin particles, absorber comprising same, and absorbent article |
WO2016021914A1 (ko) * | 2014-08-04 | 2016-02-11 | 주식회사 엘지화학 | 고흡수성 수지 및 이의 제조 방법 |
US9751995B2 (en) | 2014-08-04 | 2017-09-05 | Lg Chem, Ltd. | Superabsorbent polymer and a preparation method thereof |
JP2021509688A (ja) * | 2018-11-26 | 2021-04-01 | エルジー・ケム・リミテッド | 高吸水性樹脂およびその製造方法 |
JP7000561B2 (ja) | 2018-11-26 | 2022-01-19 | エルジー・ケム・リミテッド | 高吸水性樹脂およびその製造方法 |
US11466128B2 (en) | 2018-11-26 | 2022-10-11 | Lg Chem, Ltd. | Superabsorbent polymer and preparation method thereof |
WO2023119798A1 (ja) * | 2021-12-21 | 2023-06-29 | 住友精化株式会社 | 被覆樹脂粒子、吸水性樹脂組成物及び吸収体 |
Also Published As
Publication number | Publication date |
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TWI393726B (zh) | 2013-04-21 |
WO2007070776A2 (en) | 2007-06-21 |
US7906585B2 (en) | 2011-03-15 |
KR101297064B1 (ko) | 2013-08-19 |
CN101326234B (zh) | 2012-07-18 |
JP5557268B2 (ja) | 2014-07-23 |
EP1969053A2 (en) | 2008-09-17 |
TW200728327A (en) | 2007-08-01 |
EP1969053B1 (en) | 2014-05-07 |
US7812082B2 (en) | 2010-10-12 |
JP2014080617A (ja) | 2014-05-08 |
CN101326234A (zh) | 2008-12-17 |
WO2007070776A3 (en) | 2007-08-09 |
US20070135554A1 (en) | 2007-06-14 |
US20080021130A1 (en) | 2008-01-24 |
KR20080092341A (ko) | 2008-10-15 |
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