JP2020520390A - 高吸水性樹脂の製造方法 - Google Patents
高吸水性樹脂の製造方法 Download PDFInfo
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- JP2020520390A JP2020520390A JP2019548022A JP2019548022A JP2020520390A JP 2020520390 A JP2020520390 A JP 2020520390A JP 2019548022 A JP2019548022 A JP 2019548022A JP 2019548022 A JP2019548022 A JP 2019548022A JP 2020520390 A JP2020520390 A JP 2020520390A
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Abstract
Description
本出願は、2018年4月3日付の韓国特許出願第10−2018−0038632号に基づく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。
水溶性エチレン系不飽和単量体および重合開始剤を含むモノマー組成物に熱重合または光重合を進行させて含水ゲル状重合体を製造する段階;
前記含水ゲル状重合体を乾燥および粉砕し、150μm以下の粒径を有する微粉、および150μm超過850μm以下の粒径を有する正常粒子に分級する段階;および
前記微粉を線速度6.5〜14.5m/sで撹拌しながら水と混合し、再造粒して微粉再造粒体を製造する段階;を含み、
前記微粉と水の混合時、前記水を微粉に対して2回以上分割投入する、高吸水性樹脂の製造方法を提供する。
水溶性エチレン系不飽和単量体および重合開始剤を含むモノマー組成物に熱重合または光重合を進行させて含水ゲル状重合体を製造する段階(段階1);
前記含水ゲル状重合体を乾燥および粉砕して150μm以下の粒径を有する微粉、および150μm超過850μm以下の粒径を有する正常粒子に分級する段階(段階2);および
前記微粉を線速度6.5〜14.5m/sで撹拌しながら水と混合し、再造粒して微粉再造粒体を製造する段階(段階3);を含み、
前記微粉と水の混合時、前記水を微粉に対して2回以上分割投入する。
(製造例1)
アクリル酸100g、架橋剤としてポリエチレングリコールジアクリレート0.3g、重合開始剤として過硫酸ナトリウム0.033g、苛性ソーダ(NaOH)38.9g、および水103.9gの比率で混合して単量体の濃度が50重量%の単量体混合物を準備した。
(実施例1−1)
前記製造例1で製造された、150μm以下の粒径を有する微粉100gをミキサに入れて、線速度8.51m/sで撹拌しながら、水77gを1次投入し、2秒後に水33gを2次投入し、撹拌した。この時、前記水の2次投入完了時点から2次凝集が起こるまでの時間を測定し、微粉再造粒体がひとかたまりとなって、ミキサの負荷が増加した後、直ちにミキサの撹拌を止めた。2次凝集形成時間は13秒であった。
撹拌後、結果として得られた微粉再造粒体を強制循環型乾燥機に投入した後、180℃の温度で60分間乾燥して微粉再造粒体を回収した。
前記実施例1−1において、微粉撹拌時の線速度を12.8m/sにすることを除けば、前記実施例1−1と同様の方法で行って微粉再造粒体を回収した。2次凝集形成時間は7秒であった。
前記実施例1−1において、微粉撹拌時の線速度を4.25m/sにすることを除けば、前記実施例1−1と同様の方法で行って微粉再造粒体を回収した。2次凝集形成時間は58秒であった。
前記実施例1−1において、微粉撹拌時の線速度を16.6m/sにすることを除けば、前記実施例1−1と同様の方法で行って微粉再造粒体を回収した。2次凝集形成時間は5秒であった。
前記製造例1で製造された、150μm以下の粒径を有する微粉100gをミキサに入れて、線速度8.51m/sで撹拌しながら、SDS(sodium dodecyl sulfate)0.1重量%を添加した水溶液3.7gと、水74.4gを1次投入し、2秒後に水31.9gを2次投入し、撹拌した。この時、前記水の2次投入完了時点から2次凝集が起こるまでの時間を測定し、微粉再造粒体がひとかたまりとなって、ミキサの負荷が増加した後、直ちにミキサの撹拌を止めた。2次凝集形成時間は23秒であった。
前記実施例2−1において、微粉撹拌時の線速度を12.8m/sにすることを除けば、前記実施例2−1と同様の方法で行って微粉再造粒体を回収した。2次凝集形成時間は10秒であった。
前記実施例2−1において、水の投入時、1次で31.9gを投入し、2秒後に2次で74.4gを投入することを除けば、前記実施例2−1と同様の方法で行って微粉再造粒体を回収した。2次凝集形成時間は18秒であった。
前記実施例2−1において、水の投入時、1次で35.4gを投入し、2秒後に2次で35.4gを投入し、2秒後に3次で35.4gを投入することを除けば、前記実施例2−1と同様の方法で行って微粉再造粒体を回収した。2次凝集形成時間は19秒であった。
前記実施例1−1において、水の投入時、1次で56gを投入し、2秒後に2次で54gを投入することを除けば、前記実施例1−1と同様の方法で行って微粉再造粒体を回収した。2次凝集形成時間は13秒であった。
前記実施例2−1において、微粉撹拌時の線速度を4.25m/sにすることを除けば、前記実施例2−1と同様の方法で行って微粉再造粒体を回収した。2次凝集形成時間は85秒であった。
前記実施例2−1において、微粉撹拌時の線速度を16.6m/sにすることを除けば、前記実施例2−1と同様の方法で行って微粉再造粒体を回収した。2次凝集形成時間は8秒であった。
前記実施例2−1において、水を一括投入することを除けば、前記実施例2−1と同様の方法で行って微粉再造粒体を回収した。2次凝集形成時間は11秒であった。
前記製造例1で製造された、150μm以下の粒径を有する微粉100gをミキサに入れて、線速度4.25m/sで撹拌しながら、水110gを一括投入し、撹拌した。この時、前記水投入完了時点から2次凝集が起こるまでの時間を測定し、微粉再造粒体がひとかたまりとなって、ミキサの負荷が増加した後、直ちにミキサの撹拌を止めた。2次凝集形成時間は28秒であった。
前記比較例3−1において、微粉撹拌時の線速度を8.51m/sにすることを除けば、前記比較例3−1と同様の方法で行って微粉再造粒体を回収した。2次凝集形成時間は9秒であった。
前記比較例3−1において、微粉撹拌時の線速度を12.8m/sにすることを除けば、前記比較例3−1と同様の方法で行って微粉再造粒体を回収した。2次凝集形成時間は4秒であった。
(実施例3−1)
前記実施例1−1で製造した微粉再造粒体を、前記製造例1の微粉の製造過程で重合製造した含水ゲル状重合体と20:80の重量比で混合後、チョッピングし、乾燥した後、roll mill粉砕し、ASTM規格の標準網篩で分級して150μm以下の再造粒体微粉と、150μm超過850μm以下の粒径を有する再造粒体正常粒子に分級した。
前記実施例3−1において、実施例1−1で製造した微粉再造粒体の代わりに、実施例1−2、および実施例2−1〜実施例2−5で製造した微粉再造粒体をそれぞれ用いることを除けば、前記実施例3−1と同様の方法で行って高吸水性樹脂を製造した。
前記実施例3−1において、実施例1−1で製造した微粉再造粒体の代わりに、比較例1−1で製造した微粉再造粒体を用いることを除けば、前記実施例3−1と同様の方法で行って高吸水性樹脂を得た。
前記実施例3−1において、実施例1−1で製造した微粉再造粒体の代わりに、比較例1−2、比較例2−1〜2−3、および比較例3−1〜3−3で製造した微粉再造粒体をそれぞれ用いることを除けば、前記実施例3−1と同様の方法で行って高吸水性樹脂を製造した。
前記実施例1−1〜2−2、そして比較例1−1〜3−3による微粉再造粒体の製造時、撹拌線速度に応じた2次凝集形成時間を比較した。その結果を図1に示した。
前記実施例1−1による微粉再造粒体の製造時、撹拌時間に応じたミキサの内部状態および微粉再造粒体の形状を観察した。その結果を図2に示した。
前記実施例1−1と同様の方法で行って微粉再造粒体を製造するが、撹拌時間を5s、10s、および20sに変化させ、製造される微粉再造粒体に対する物性変化の観察により撹拌時間が微粉再造粒体に及ぼす影響を確認した。
このように得られた各質量を利用して、次の数式1によりCRC(g/g)を算出して保水能を確認した。
[数式1]
CRC(g/g)={[W2(g)−W1(g)]/W0(g)}−1
前記数式1中、
W0(g)は、微粉再造粒体の初期重量(g)であり、
W1(g)は、微粉再造粒体を用いず、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の重量であり、
W2(g)は、常温で0.9重量%生理食塩水に微粉再造粒体を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、微粉再造粒体を含んで測定した装置の重量である。
前記実施例1−1〜1−2および比較例1−1による微粉再造粒体の製造時、撹拌線速度に応じた2次凝集形成時間の変化および製造される微粉再造粒体の物性変化を観察した。
前記実施例1−1、2−1、2−3、2−4、2−5、および比較例3−2による微粉再造粒体の製造時、同一の線速度の条件下、水の分割投入および投入量に応じた2次凝集形成時間の変化を観察した。その結果を下記表3に示した。
前記実施例3−1で製造した高吸水性樹脂に対して、保水能(CRC)、0.3AUP、およびvortexをそれぞれ測定した。
直径150mmのペトロ皿の内側に直径90mmおよび厚さ5mmのガラスフィルタを置き、0.9重量%塩化ナトリウムで構成された生理食塩水をガラスフィルタの上面と同一レベルとなるようにした。その上に直径90mmのろ過紙1枚を載せた。ろ過紙の上に前記測定装置を載せ、液を荷重下で1時間吸収させた。1時間後に測定装置を持ち上げて、その重量W4(g)を測定した。
得られた各質量を利用して、次の数式3により加圧吸水能(g/g)を算出した。
[数式3]
AUP(g/g)=[W4(g)−W3(g)]/W0(g)
(3)吸水速度(Vortex)
50ml食塩水を100mlビーカーにマグネチックバーと一緒に入れて、撹拌機を用いて撹拌速度を600rpmに指定した。撹拌されている食塩水に、前記実施例3−1で製造した高吸水性樹脂2.0gを入れると同時に時間を測定した。ビーカー内に渦巻きが無くなる時点で時間の測定を終了した。
Claims (10)
- 水溶性エチレン系不飽和単量体および重合開始剤を含むモノマー組成物に熱重合または光重合を進行させて含水ゲル状重合体を製造する段階;
前記含水ゲル状重合体を乾燥および粉砕し、150μm以下の粒径を有する微粉、および150μm超過850μm以下の粒径を有する正常粒子に分級する段階;および
前記微粉を線速度6.5〜14.5m/sで撹拌しながら水と混合し、再造粒して微粉再造粒体を製造する段階を含み、
前記微粉と水の混合時、前記水を微粉に対して2回以上分割投入する、高吸水性樹脂の製造方法。 - 前記微粉と水の混合時、水は2回分割投入され、投入される水の総量に対して、50重量%超過〜90重量%以下が1次投入され、残部が2次投入される、請求項1に記載の高吸水性樹脂の製造方法。
- 前記微粉と水の混合時、水は、微粉100重量部に対して、80〜150重量部で混合される、請求項1に記載の高吸水性樹脂の製造方法。
- 前記微粉と水の混合時、水溶性高分子および界面活性剤のうちの1種以上の混合安定化剤がさらに添加される、請求項1に記載の高吸水性樹脂の製造方法。
- 前記混合安定化剤は、微粉100重量部に対して、0.001〜1重量部で投入される、請求項4に記載の高吸水性樹脂の製造方法。
- 前記水溶性高分子は、ポリエチレングリコール、ポリエチレンオキシド、ポリビニルピロリドン、ポリビニルアルコール、ポリアクリルアミド、ポリアクリル酸、ポリスチレンスルホン酸、ポリケイ酸、ポリリン酸、ポリエチレンスルホン酸、ポリビニルフェノール、ポリビニルフェニルスルホン酸、ポリエチレンリン酸、ポリエチレンアミド、ポリアミン、ポリアミドアミン、デンプン、ゴム、およびセルロースからなる群より選択されるいずれか1または2以上を含む、請求項4に記載の高吸水性樹脂の製造方法。
- 前記界面活性剤は、ソジウムドデシルスルフェート、ジイソオクチルソジウムスルホスクシネート塩、ソジウムテトラデシルスルフェート、ソジウムヘキサデシルスルフェート、ソジウムドデシルベンゼンスルフェート、キシレンスルホネート、ソジウムオレアート、4−n−デシルベンゼンスルホネート、ソジウムラウレート、4−ドデシルベンゼンスルホン酸、ドデシルアミンヒドロクロライド、ドデシルトリメチルアンモニウムクロライド、4−n−オクチルベンゼンスルホネート、エトキシ化スルホネート、デシルベンゼンスルホネート、ポタシウムオレアート、n−デシルベンゼンスルホネート、アルキルトリメチルアンモニウムブロミド、ドデシルアミン、テトラデシルトリメチルアンモニウムクロライド、ドデシルポリサッカライドグリコシド、シクロデキストリン、グリコリピッド、リポプロティン−リポペプチド、ホスホリピッド、パラ−トルエンスルホン酸、およびトリシロキサンからなる群より選択されるいずれか1または2以上を含む、請求項4に記載の高吸水性樹脂の製造方法。
- 前記混合安定化剤は、ポリエチレングリコールおよびソジウムドデシルスルフェートのうちの少なくとも1種を含む、請求項4に記載の高吸水性樹脂の製造方法。
- 前記微粉再造粒体を前記段階1で製造した含水ゲル状重合体と混合後、乾燥および粉砕して150μm以下の粒径を有する再造粒体微粉、および150μm超過850μm以下の粒径を有する再造粒体正常粒子に分級する段階をさらに含む、請求項1に記載の高吸水性樹脂の製造方法。
- 前記再造粒体正常粒子を表面架橋剤と混合して表面架橋する段階をさらに含む、請求項9に記載の高吸水性樹脂の製造方法。
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KR101960043B1 (ko) * | 2015-11-03 | 2019-07-04 | 주식회사 엘지화학 | 고흡수성 수지의 제조 방법 |
KR101853401B1 (ko) | 2016-03-11 | 2018-04-30 | 주식회사 엘지화학 | 고흡수성 수지의 제조 방법, 및 고흡수성 수지 |
KR20180003815A (ko) * | 2016-07-01 | 2018-01-10 | 한화케미칼 주식회사 | 고흡수성 수지 제조 방법 |
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JPH11106514A (ja) * | 1997-06-18 | 1999-04-20 | Nippon Shokubai Co Ltd | 吸水性樹脂造粒物の製造方法 |
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WO2022075289A1 (ja) * | 2020-10-06 | 2022-04-14 | 住友精化株式会社 | 吸水性樹脂粒子の製造方法 |
WO2022075256A1 (ja) * | 2020-10-06 | 2022-04-14 | 住友精化株式会社 | 吸水性樹脂粒子の製造方法 |
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EP3730539B1 (en) | 2023-07-05 |
EP3730539A4 (en) | 2021-04-21 |
KR20190115661A (ko) | 2019-10-14 |
CN110557949B (zh) | 2022-06-24 |
WO2019194399A1 (ko) | 2019-10-10 |
CN110557949A (zh) | 2019-12-10 |
US11161942B2 (en) | 2021-11-02 |
JP7008718B2 (ja) | 2022-01-25 |
EP3730539A1 (en) | 2020-10-28 |
US20200247960A1 (en) | 2020-08-06 |
KR102555381B1 (ko) | 2023-07-12 |
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