JP2014515413A - 吸水性ポリマー粒子の連続的な製造法 - Google Patents
吸水性ポリマー粒子の連続的な製造法 Download PDFInfo
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Classifications
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/18—Suspension polymerisation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
Description
a)少なくとも部分的に中和されていてよい、少なくとも1種のエチレン性不飽和の酸基含有モノマー、
b)少なくとも1種の架橋剤、
c)少なくとも1種の開始剤、
d)任意に、a)で挙げられるモノマーと共重合可能な1種以上のエチレン性不飽和モノマー及び
e)任意に、1種以上の水溶性ポリマー
を含むモノマー溶液又はモノマー懸濁液を連続的な重合反応器中で重合してポリマーゲルを取得し、得られたポリマーゲルを乾燥し、乾燥されたポリマーゲルを細分化してポリマー粒子を取得し、かつ得られたポリマー粒子を分級することによって、吸水性ポリマー粒子を連続的に製造する方法において、開始剤c)の使用量及び/又は重合を引き起こすために任意に使用される紫外線の強度を、重合反応器の運転開始後の最初の120分以内に少なくとも10%下げることを特徴とする方法によって解決された。
吸水性ポリマー粒子は、モノマー溶液又はモノマー懸濁液の重合によって製造され、かつ通常は水不溶性である。
以下に記載した"WSP"で表記される標準試験法は、"Worldwide Strategic Partners"EDANA(欧州不織布協会)(Avenue Eugene Plasky 157,1030 Brussels,Belgium,www.edana.org)及びINDA(米国不織布協会)(1100 Crescent Green,Cary,North Carolina 27518,U.S.A.,www.inda.org)により共同で出版された"Standard Test Methods for the Nonwovens Industry",2005 editionに記載されている。この刊行物は、EDANAからもINDAからも入手可能である。
遠心分離保持容量(CRC)は、EDANAにより推奨される試験法No.WSP 241.2−05 "Fluid Retention Capacity in Saline,After Centrifugation"に従って測定する。
吸水性ポリマー粒子の抽出可能な構成成分の含量は、EDANAによって推奨される試験法No.WSP 270.2−05 "Extractable"に従って測定する。
例1
アクリル酸75.7g、アクリル酸ナトリウム水溶液681.7g(37.3質量%)、脱イオン水235.3g及び3箇所でエトキシ化されたグリセリントリアクリレート1.35g(約85質量%)より成る、約15℃に冷却した溶液から、30分間窒素を導入することによって空気中酸素を除去した。2リットルのプラスチック容器中で、ペルオキソ二硫酸ナトリウム水溶液3.0g(25.2質量%)、アスコルビン酸水溶液4.0g(0.40質量%)及び過酸化水素水溶液5.0g(0.08質量%)の添加によって重合を引き起こした。得られたゲルを、ミートグラインダで細分化し、次いで空気循環式乾燥キャビネット内で150℃にて60分間乾燥し、ロールミルで粉砕し、かつ150〜850μmの粒径範囲に篩分することによって調節した。
例1と同じように処理を行った。ペルオキソ二硫酸ナトリウム、アスコルビン酸及び過酸化水素の量は、それぞれ半分に下げた。得られたポリマー粒子を分析した。結果は、表1にまとめている。
アクリル酸105.1g、アクリル酸ナトリウム水溶液683.3g(37.3質量%)、脱イオン水204.1g及び3箇所でエトキシ化されたグリセリントリアクリレート1.50g(約85質量%)より成る、約15℃に冷却した溶液から、30分間窒素を導入することによって空気中酸素を除去した。2リットルのプラスチック容器中で、過硫酸ナトリウム水溶液3.0g(28.0質量%)、アスコルビン酸水溶液2.0g(0.46質量%)及び過酸化水素水溶液5.0g(0.1質量%)の添加によって重合を引き起こした。反応混合物は、12分後に100℃の温度に達した。得られたゲルを、ミートグラインダで細分化し、次いで空気循環式乾燥キャビネット内で150℃にて60分間乾燥し、ロールミルで粉砕し、かつ150〜850μmの粒径範囲に篩分することによって調整した。
例3と同じように処理を行った。ペルオキソ二硫酸ナトリウム、アスコルビン酸及び過酸化水素の量は、それぞれ半分に下げた。反応混合物は、18分後に100℃の温度に達した。得られたポリマー粒子を分析した。結果は、表2にまとめている。
アクリル酸39.0g、アクリル酸ナトリウム水溶液349.1g(37.3質量%)、脱イオン水105.2g及び3箇所でエトキシ化されたグリセリントリアクリレート0.70g(約85質量%)より成る、約15℃に冷却した溶液から、30分間窒素を導入することによって空気中酸素を除去した。1リットルのプラスチック容器中で、過硫酸ナトリウム水溶液3.0g(20.0質量%)、アスコルビン酸水溶液1.5g(0.84質量%)及び過酸化水素水溶液1.5g(0.74質量%)の添加によって重合を引き起こした。得られたゲルを、ミートグラインダで細分化し、次いで空気循環式乾燥キャビネット内で150℃にて60分間乾燥し、ロールミルで粉砕し、かつ150〜850μmの粒径範囲に篩分することによって調整した。
例5を繰り返した。結果は、表3にまとめている。
例5と同じように処理を行った。ペルオキソ二硫酸ナトリウム、アスコルビン酸及び過酸化水素の量は、それぞれ3分の2に下げた。得られたポリマー粒子を分析した。結果は、表3にまとめている。
例7を繰り返した。結果は、表3にまとめている。
例5と同じように処理を行った。ペルオキソ二硫酸ナトリウム、アスコルビン酸及び過酸化水素の量は、それぞれ3分の1に下げた。得られたポリマー粒子を分析した。結果は、表3にまとめている。
例9を繰り返した。得られた生成物を粉砕することはできなかった。
Claims (10)
- a)少なくとも部分的に中和されていてよい、少なくとも1種のエチレン性不飽和の酸基含有モノマー、
b)少なくとも1種の架橋剤、
c)少なくとも1種の開始剤、
d)任意に、a)で挙げられるモノマーと共重合可能な1種以上のエチレン性不飽和モノマー及び
e)任意に、1種以上の水溶性ポリマー
を含むモノマー溶液又はモノマー懸濁液を連続的な重合反応器中で重合してポリマーゲルを取得し、得られたポリマーゲルを乾燥し、乾燥されたポリマーゲルを細分化してポリマー粒子を取得し、かつ得られたポリマー粒子を分級することによって、吸水性ポリマー粒子を連続的に製造する方法において、開始剤c)の使用量及び/又は重合を引き起こすために任意に使用される紫外線の強度を、重合反応器の運転開始後の最初の120分以内に少なくとも10%下げることを特徴とする方法。 - 前記開始剤c)の使用量を、前記重合反応器の運転開始後の最初の30分以内に少なくとも40%下げることを特徴とする、請求項1記載の方法。
- 前記重合反応器を、前記重合の運転開始前に少なくとも50℃に予熱することを特徴とする、請求項1又は2記載の方法。
- 前記重合反応器中での平均滞留時間が5〜120分であることを特徴とする、請求項1から3までのいずれか1項記載の方法。
- 前記重合反応器が混練反応器であることを特徴とする、請求項1から4までのいずれか1項記載の方法。
- 前記重合反応器がベルト型反応器であることを特徴とする、請求項1から4までのいずれか1項記載の方法。
- 前記吸水性ポリマー粒子を、表面後架橋し、任意にコーティングし、かつ任意に分級することを特徴とする、請求項1から6までのいずれか1項記載の方法。
- 前記モノマーa)の少なくとも50モル%が、部分的に中和されたアクリル酸であることを特徴とする、請求項1から7までのいずれか1項記載の方法。
- 前記モノマーa)の少なくとも25〜85モル%が中和されていることを特徴とする、請求項1から8までのいずれか1項記載の方法。
- 前記吸水性ポリマー粒子が、少なくとも15g/gの遠心分離保持容量を有することを特徴とする、請求項1から9までのいずれか1項記載の方法。
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EP2714103B1 (de) | 2019-08-21 |
WO2012159949A1 (de) | 2012-11-29 |
CN103561781A (zh) | 2014-02-05 |
JP2017101261A (ja) | 2017-06-08 |
CN103561781B (zh) | 2016-06-29 |
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