JP6449902B2 - 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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- JP6449902B2 JP6449902B2 JP2016557857A JP2016557857A JP6449902B2 JP 6449902 B2 JP6449902 B2 JP 6449902B2 JP 2016557857 A JP2016557857 A JP 2016557857A JP 2016557857 A JP2016557857 A JP 2016557857A JP 6449902 B2 JP6449902 B2 JP 6449902B2
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- superabsorbent resin
- producing
- polymer
- superabsorbent
- water
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- LSHROXHEILXKHM-UHFFFAOYSA-N n'-[2-[2-[2-(2-aminoethylamino)ethylamino]ethylamino]ethyl]ethane-1,2-diamine Chemical compound NCCNCCNCCNCCNCCN LSHROXHEILXKHM-UHFFFAOYSA-N 0.000 description 1
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- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
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Classifications
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
- B01J20/267—Cross-linked polymers
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/42—Use of materials characterised by their function or physical properties
- A61L15/60—Liquid-swellable gel-forming materials, e.g. super-absorbents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3021—Milling, crushing or grinding
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Description
a)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単量体組成物を熱重合または光重合して、含水ゲル状重合体を用意するステップと、b)前記含水ゲル状重合体を乾燥するステップと、c)前記乾燥した含水ゲル状重合体を粉砕するステップと、d)前記粉砕された含水ゲル状重合体に、下記i)乃至ii)の特性を有する粒子と表面架橋剤を添加するステップと、e)表面架橋反応を行うステップとを含む高吸水性樹脂の製造方法を提供する。
i)300〜1500m2/gのBET比表面積(specific surface area)、
ii)50%以上の孔隙率(porosity)
a)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単量体組成物を熱重合または光重合して、含水ゲル状重合体を用意するステップと、b)前記含水ゲル状重合体を乾燥するステップと、c)前記乾燥した含水ゲル状重合体を粉砕するステップと、d)前記粉砕された含水ゲル状重合体に、下記i)乃至ii)の特性を有する粒子と表面架橋剤を添加するステップと、e)表面架橋反応を行うステップとを含む。
i)300〜1500m2/gのBET比表面積(specific surface area)、
ii)50%以上の孔隙率(porosity)
i)300〜1500m2/gのBET比表面積(specific surface area)、
ii)50%以上の孔隙率(porosity)
以下、本発明を実施例に基づいてより詳細に説明するが、下記に開示される本発明の実施形態はあくまで例示であって、本発明の範囲はこれらの実施形態に限定されない。本発明の範囲は、特許請求の範囲に示され、なおかつ特許請求の範囲の記録と均等な意味および範囲内でのすべての変更を含んでいる。また、以下の実施例、比較例において、含有量を示す「%」および「部」は、特に言及しない限り、質量基準である。
製造例:含水ゲル状重合体の製造
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、開始剤としてジフェニル(2,4,6−トリメチルベンゾイル)−ホスフィンオキシド0.033g、苛性ソーダ(NaOH)38.9g、および水103.9gの比率で混合して、単量体混合物を用意した。
[実施例1]
前記製造例によって用意された含水ゲル状重合体を5*5mmの大きさに切断して、170℃の温度の熱風乾燥機で2時間乾燥し、ピンミル粉砕機で粉砕した後、篩(sieve)を用いて、粒径サイズが150〜850μmの高吸水性樹脂を得た。前記高吸水性樹脂250gに、多孔性超疎水性微細粒子silica Aerogel(AeroZelTM、JIOS社)0.15gを1000RPMで60秒間混合した後、表面架橋剤としてエチレンカーボネート0.75gと水6.75gで構成された液状混合物を投与した後、60秒間混合した。以後、前記混合物を190℃で60分間反応して未粉砕高吸水性樹脂を得て、再び、前記未粉砕高吸水性樹脂の粉砕前の粒径を測定し、ピンミル粉砕機で粉砕した後、篩を用いて、粒径サイズが150〜850μmの高吸水性樹脂を得た。前記使用したAerogelの粒径は30nmであり、500m2/gのBET比表面積を有し、水に対する接触角は150゜であり、孔隙率は95%であった。
Silica Aerogelの量を0.25g使用したことを除いては、実施例1と同様の方法で行って高吸水性樹脂を得た。
液状混合物中の水の量を11.75g使用したことを除いては、実施例1と同様の方法で行って高吸水性樹脂を得た。
Silica Aerogelの量を0.25g、液状混合物中の水の量を11.75g使用したことを除いては、実施例1と同様の方法で行って高吸水性樹脂を得た。
微細粒子としてREOLOSIL DM−30Sを使用したことを除いては、実施例1と同様の方法で行って高吸水性樹脂を得た。前記使用したREOLOSIL DM−30Sの粒径は7nmであり、230m2/gのBET比表面積を有し、水に対する接触角は
135゜であり、孔隙率は20%以下であり、測定方法は実施例1と同様である。
微細粒子としてREOLOSIL DM−30Sを0.25g使用したことを除いては、比較例1と同様の方法で行って高吸水性樹脂を得た。
微細粒子としてREOLOSIL DM−30Sを、液状混合物中の水の量を11.75g使用したことを除いては、比較例1と同様の方法で行って高吸水性樹脂を得た。
微細粒子としてREOLOSIL DM−30Sを0.25g、液状混合物中の水の量を11.75g使用したことを除いては、比較例1と同様の方法で行って高吸水性樹脂を得た。
微細粒子を使用しないことを除いては、実施例1と同様の方法で行って高吸水性樹脂を得た。
液状混合物中の水の量を11.75g使用したことを除いては、比較例5と同様の方法で行って高吸水性樹脂を得た。
前記比較例1〜比較例6および実施例1〜実施例4による高吸水性樹脂の物性を評価するために、下記のような試験を行った。
前記比較例1〜比較例6および実施例1〜実施例4で用意された高吸水性樹脂それぞれ
に対する保水能を測定した。保水能の測定は、EDANA法WSP241.3を基準とした。用意された高吸水性樹脂中、粒径150〜850μmまたは既分級試料0.2gをティーバッグに入れて、0.9%塩水溶液に30分間沈殿させた。以後、250G(gravity)の遠心力で3分間脱水した後、塩水溶液が吸収された量を測定した。
前記比較例1〜比較例6および実施例1〜実施例4で用意された高吸水性樹脂それぞれに対する加圧吸水能を測定した。加圧吸水能の測定は、EDANA法WSP242.3を基準とした。用意された高吸水性樹脂中、粒径150〜850μmまたは既分級試料0.9gをEDATAで規定するシリンダに入れて、ピストンと錘で0.7psiの圧力を加えた後に、0.9%塩水溶液を60分間吸収した量を測定した。
前記比較例1〜比較例6および実施例1〜実施例4の未粉砕高吸水性樹脂に対する粒径を測定した。高吸水性樹脂の粒径の測定は、EDANA法WSP220.3を基準とした。高吸水性樹脂100gを850μm、600μm、300μm、150μm、PanのMeshに区分して、1.44mmの振幅、振動数50Hzで10分間振動した後、各篩の上部に滞留量の比率で含有量を測定した。
脂は、比較例5により製造された高吸水性樹脂より粒径の小さい側に分布するもので、粉砕工程がないにもかかわらず、850μm以下の粒径が75%程度維持されることにより、加工性が増加することを確認することができる。
Claims (17)
- a)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単量体組成物を熱重合または光重合して、含水ゲル状重合体を用意するステップと、
b)前記含水ゲル状重合体を乾燥するステップと、
c)前記乾燥した含水ゲル状重合体を粉砕するステップと、
d)前記粉砕された含水ゲル状重合体に、シリカ、アルミナ、炭素(Carbon)、およびチタニア(TiO 2 )からなる群より選択される1種以上からなり且つ下記i)乃至iv)の特性を有する粒子と表面架橋剤を添加するステップと、
e)表面架橋反応を行うステップとを含む高吸水性樹脂の製造方法。
i)2nm〜50μmの粒径、
ii)300〜1500m2/gのBET比表面積(specific surface area)、
iii)水に対する125゜以上の接触角、
iv)50%以上の孔隙率(porosity) - 前記粒子は、500〜1500m2/gのBET比表面積(specific surface area)を有することを特徴とする請求項1に記載の高吸水性樹脂の製造方法。
- 前記粒子は、700〜1500m2/gのBET比表面積(specific surface area)を有することを特徴とする請求項1に記載の高吸水性樹脂の製造方法。
- 前記粒子は、水に対する接触角が140゜以上の超疎水性を有することを特徴とする請求項1に記載の高吸水性樹脂の製造方法。
- 前記粒子は、水に対する接触角が145゜以上の超疎水性を有することを特徴とする請求項1に記載の高吸水性樹脂の製造方法。
- 前記粒子は、90%以上の孔隙率(porosity)を有することを特徴とする請求項1に記載の高吸水性樹脂の製造方法。
- 前記粒子は、高吸水性樹脂100重量部に対して、0.001〜1重量部含まれることを特徴とする請求項1に記載の高吸水性樹脂の製造方法。
- 前記ステップb)の乾燥ステップの前に、含水ゲル状重合体を粒径1mm〜15mmに粉砕するステップをさらに含むことを特徴とする請求項1に記載の高吸水性樹脂の製造方法。
- 前記ステップb)の乾燥ステップは、150℃〜250℃の温度で行われることを特徴とする請求項1に記載の高吸水性樹脂の製造方法。
- 前記ステップc)の粉砕ステップは、含水ゲル状重合体を粒径150〜850μmに粉砕することを特徴とする請求項1に記載の高吸水性樹脂の製造方法。
- 前記ステップd)の表面架橋剤は、多価アルコール化合物;エポキシ化合物;ポリアミン化合物;ハロエポキシ化合物;ハロエポキシ化合物の縮合生成物;オキサゾリン化合物;モノ−、ジ−またはポリオキサゾリジノン化合物;環状ウレア化合物;多価金属塩;およびアルキレンカーボネート化合物からなる群より選択されるいずれか1つ以上であることを特徴とする請求項1に記載の高吸水性樹脂の製造方法。
- 前記ステップd)の表面架橋剤は、粉砕された重合体100重量部に対して、0.001〜5重量部が添加されることを特徴とする請求項1に記載の高吸水性樹脂の製造方法。
- 前記ステップd)において、前記表面架橋剤を添加するステップにおける前記重合体の表面温度は、60〜90℃であることを特徴とする請求項1に記載の高吸水性樹脂の製造方法。
- 前記ステップd)において、添加される表面架橋剤の温度は、5〜40℃であることを特徴とする請求項1に記載の高吸水性樹脂の製造方法。
- 前記ステップe)において、前記表面架橋反応は、10分〜120分間行われることを特徴とする請求項1に記載の高吸水性樹脂の製造方法。
- 前記ステップe)において、スチーム、電気、紫外線、および赤外線からなる熱源の群より選択されるいずれか1つ以上を照射して昇温することを特徴とする請求項1に記載の高吸水性樹脂の製造方法。
- 前記ステップe)の表面架橋反応ステップの後に、高吸水性樹脂を150〜850μmの粒径に再び粉砕するステップをさらに含むことを特徴とする請求項1に記載の高吸水性樹脂の製造方法。
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KR101700907B1 (ko) * | 2013-12-10 | 2017-01-31 | 주식회사 엘지화학 | 고흡수성 수지의 제조 방법 |
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CN105722863A (zh) | 2016-06-29 |
EP3078678A4 (en) | 2016-10-12 |
EP3078678B1 (en) | 2017-08-30 |
EP3078678A1 (en) | 2016-10-12 |
US20160271584A1 (en) | 2016-09-22 |
JP2016540106A (ja) | 2016-12-22 |
US9700871B2 (en) | 2017-07-11 |
KR20150064649A (ko) | 2015-06-11 |
CN105722863B (zh) | 2017-05-24 |
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