JP2016533423A - 高吸水性樹脂およびその製造方法 - Google Patents
高吸水性樹脂およびその製造方法 Download PDFInfo
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- JP2016533423A JP2016533423A JP2016545697A JP2016545697A JP2016533423A JP 2016533423 A JP2016533423 A JP 2016533423A JP 2016545697 A JP2016545697 A JP 2016545697A JP 2016545697 A JP2016545697 A JP 2016545697A JP 2016533423 A JP2016533423 A JP 2016533423A
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- 238000002791 soaking Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229920001059 synthetic polymer Polymers 0.000 description 1
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- LDHQCZJRKDOVOX-UHFFFAOYSA-N trans-crotonic acid Natural products CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 description 1
- VPYJNCGUESNPMV-UHFFFAOYSA-N triallylamine Chemical compound C=CCN(CC=C)CC=C VPYJNCGUESNPMV-UHFFFAOYSA-N 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
- 238000004078 waterproofing Methods 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
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- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
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- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
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Abstract
Description
前記乾燥された重合体を粉砕する段階と、
粉砕された重合体に表面架橋剤および水を含む表面架橋溶液を混合して180〜200℃で加熱することによって表面架橋反応を行う段階と、
を含む高吸水性樹脂の製造方法を提供する。
実施例1
アクリル酸(水溶性エチレン系不飽和単量体)100重量部、アクリル酸100重量部を基準に、potassium igacure 651(光重合開始剤)0.03重量部およびポリエチレングリコールジアクリレート(架橋剤)0.3重量部を含むモノマー組成物を準備した。前記モノマー組成物を10cmの幅、2mの長さを有し、50cm/minの速度で回転する回転式ベルト上に、500mL/min〜2,000mL/minの供給速度で供給した。
前記実施例1の重合体100重量部に対して、エチレンカーボネート0.4重量部、メタノール5重量部、水4重量部を混合してコンベクションオーブンを用いて200℃で40分間表面処理反応を行ったことを除いては、実施例1と同様な方法で高吸水性樹脂を製造した。
実施例1の重合体100重量部に対して、エチレンカーボネート0.4重量部、メタノール5重量部、水4重量部を混合してコンベクションオーブンを用いて180℃で80分間表面処理反応を行ったことを除いては、実施例1と同様な方法で高吸水性樹脂を製造した。
アクリル酸(水溶性エチレン系不飽和単量体)100重量部、アクリル酸100重量部を基準に、potassium igacure 651(光重合開始剤)0.03重量部、ポリエチレングリコールジアクリレート(架橋剤)0.5重量部、および1,6−ヘキサンジオールジアクリレート(架橋剤)0.1重量部を含むモノマー組成物を準備した。前記モノマー組成物を10cmの幅、2mの長さを有し、50cm/minの速度で回転する回転式ベルト上に、500mL/min〜2,000mL/minの供給速度で供給した。
実施例4の重合体100重量部に対して、エチレンカーボネート0.4重量部、メタノール5重量部、水4重量部を混合してコンベクションオーブンを用いて200℃で40分間表面処理反応を行ったことを除いては、実施例4と同様な方法で高吸水性樹脂を製造した。
実施例4の重合体100重量部に対して、エチレンカーボネート0.4重量部、メタノール5重量部、水4重量部を混合してコンベクションオーブンを用いて180℃で80分間表面処理反応を行ったことを除いては、実施例4と同様な方法で高吸水性樹脂を製造した。
実施例1の重合体100重量部に対して、エチレンカーボネート0.4重量部、メタノール5重量部、水4重量部を混合してコンベクションオーブンを用いて210℃で20分間表面処理反応を行ったことを除いては、実施例1と同様な方法で高吸水性樹脂を製造した。
実施例1の重合体100重量部に対して、エチレンカーボネート0.4重量部、メタノール5重量部、水4重量部を混合してコンベクションオーブンを用いて175℃で90分間表面処理反応を行ったことを除いては、実施例1と同様な方法で高吸水性樹脂を製造した。
実施例4の重合体100重量部に対して、エチレンカーボネート0.4重量部、メタノール5重量部、水4重量部を混合してコンベクションオーブンを用いて210℃で20分間表面処理反応を行ったことを除いては、実施例4と同様な方法で高吸水性樹脂を製造した。
実施例4の重合体100重量部に対して、エチレンカーボネート0.4重量部、メタノール5重量部、水4重量部を混合してコンベクションオーブンを用いて175℃で90分間表面処理反応を行ったことを除いては、実施例4と同様な方法で高吸水性樹脂を製造した。
透過率、保水能および加圧吸収能の測定比較
透過率は、文献(Buchholz, F.L. and Graham, A.T., “Modern Superabsorbent Polymer Technology, ” John Wiley and Sons(1998), page 161)に記述された方法により0.9%塩水溶液を用いて0.3psi荷重下に測定した。
透過率(sec)=時間(サンプル)−時間(高吸水性樹脂の投入なしに測定)
保水能測定は、EDANA法WSP241.2に従った。30〜50メッシュで分級したサンプル0.2gをティーバッグに入れて30分間0.9%塩水溶液に浸した後、250Gに設定された遠心分離機で3分間水を除去し、重量を測って高吸水性樹脂が保有している水の量を測定する方式で保水能を測定した。
実施例および比較例で製造された高吸水性樹脂1gを250mLの三角フラスコに入れた後、0.9%NaCl溶液200mLで25℃で500rpmで攪拌する条件により1時間膨潤(swelling)させ、溶出された溶液をフィルターペーパー(filter paper)を通過させた後、100μLを取ってGPC装置に注入して測定した。GPCは、Wyatt DAWN EOS、Wyatt Optila bDSP、Waters、Wyatt社の機器を使用し、カラムは、Ultrahydrogel Linear X2、溶媒としては、0.1MのNaNO3/0.02Mのリン酸緩衝液(phosphate buffer)を使用し、流速0.8mL/min、温度60℃の条件によりスタンダード(Standard)にポリアクリル酸(polyacrylic acid)が使用された。
実施例1の重合体100重量部に対して、エチレンカーボネート0.4重量部、メタノール5重量部、水4重量部を混合してコンベクションオーブンを用いて175℃で90分間表面処理反応を行ったことを除いては、実施例1と同様な方法で高吸水性樹脂を製造した。
実施例4の重合体100重量部に対して、エチレンカーボネート0.4重量部、メタノール5重量部、水4重量部を混合してコンベクションオーブンを用いて210℃で20分間表面処理反応を行ったことを除いては、実施例4と同様な方法で高吸水性樹脂を製造した。
実施例4の重合体100重量部に対して、エチレンカーボネート0.4重量部、メタノール5重量部、水4重量部を混合してコンベクションオーブンを用いて175℃で90分間表面処理反応を行ったことを除いては、実施例4と同様な方法で高吸水性樹脂を製造した。
実施例、参考例および比較例で製造された高吸水性樹脂1gを250mLの三角フラスコに入れた後、0.9%NaCl溶液200mLで25℃で500rpmで攪拌する条件により1時間膨潤(swelling)させ、溶出された溶液をフィルターペーパー(filter paper)を通過させた後、100μLを取ってGPC装置に注入して測定した。GPCは、Wyatt DAWN EOS、Wyatt Optila bDSP、Waters、Wyatt社の機器を使用し、カラムは、Ultrahydrogel Linear X2、溶媒としては、0.1MのNaNO3/0.02Mのリン酸緩衝液(phosphate buffer)を使用し、流速0.8mL/min、温度60℃の条件によりスタンダード(Standard)にポリアクリル酸(polyacrylic acid)が使用された。
Claims (6)
- 水溶性エチレン系不飽和単量体を重合させたベース樹脂を表面架橋させた架橋重合体、および水可溶成分を含む高吸水性樹脂であって、
前記高吸水性樹脂を1時間膨潤(swelling)させた後に測定した時、重量平均分子量が100,000〜300,000である水可溶成分の重量平均分子量(M)のログ値に対する分子量分布(dwt/d(log M))が0.9以下である、高吸水性樹脂。 - 前記高吸水性樹脂を1時間膨潤させた後に測定した時、前記水可溶成分が高吸水性樹脂全体に対して5重量%以下含まれる、請求項1に記載の高吸水性樹脂。
- 前記高吸水性樹脂は、26〜37g/gの保水能、および20〜26g/gの加圧吸収能を有する、請求項1に記載の高吸水性樹脂。
- 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行って含水ゲル状重合体を形成する段階と、
前記含水ゲル状重合体を乾燥する段階と、
前記乾燥された重合体を粉砕する段階と、
粉砕された重合体に表面架橋剤および水を含む表面架橋溶液を混合して180〜200℃で加熱することによって表面架橋反応を行う段階と、
を含む高吸水性樹脂の製造方法。 - 前記高吸水性樹脂を1時間膨潤(swelling)させた後に測定した時、重量平均分子量が100,000〜300,000である水可溶成分の重量平均分子量(M)のログ値に対する分子量分布(dwt/d(log M))が0.9以下である、請求項4に記載の高吸水性樹脂の製造方法。
- 前記高吸水性樹脂を1時間膨潤させた後に測定した時、前記水可溶成分が高吸水性樹脂全体に対して5重量%以下含まれる、請求項4に記載の高吸水性樹脂の製造方法。
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EP (1) | EP3026066A4 (ja) |
JP (1) | JP6473162B2 (ja) |
KR (1) | KR101495845B1 (ja) |
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KR101495845B1 (ko) | 2013-09-30 | 2015-02-25 | 주식회사 엘지화학 | 고흡수성 수지 및 이의 제조 방법 |
US10285866B2 (en) | 2015-01-16 | 2019-05-14 | Lg Chem, Ltd. | Super absorbent polymer |
KR20170106109A (ko) * | 2016-03-11 | 2017-09-20 | 주식회사 엘지화학 | 고흡수성 수지의 투과율 측정방법 |
KR101863350B1 (ko) * | 2016-03-31 | 2018-06-01 | 주식회사 엘지화학 | 고흡수성 수지 및 이의 제조 방법 |
KR102242700B1 (ko) * | 2016-04-20 | 2021-04-21 | 한화솔루션 주식회사 | 고흡수성 수지 및 이의 제조 방법 |
KR20180067940A (ko) | 2016-12-13 | 2018-06-21 | 주식회사 엘지화학 | 고흡수성 수지 및 이의 제조 방법 |
KR102094453B1 (ko) | 2016-12-23 | 2020-03-27 | 주식회사 엘지화학 | 고흡수성 수지 및 이의 제조 방법 |
KR102577709B1 (ko) * | 2018-01-16 | 2023-09-11 | 주식회사 엘지화학 | 고흡수성 수지의 제조 방법 |
EP3753976B1 (en) * | 2018-11-13 | 2023-08-30 | Lg Chem, Ltd. | Method for preparing super absorbent polymer |
US11578415B2 (en) | 2018-11-28 | 2023-02-14 | Twelve Benefit Corporation | Electrolyzer and method of use |
KR102251794B1 (ko) * | 2020-07-16 | 2021-05-12 | 주식회사 엘지화학 | 고흡수성 수지의 제조 방법 |
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WO2015046994A1 (ko) | 2015-04-02 |
CN105636990A (zh) | 2016-06-01 |
KR101495845B1 (ko) | 2015-02-25 |
US9486778B2 (en) | 2016-11-08 |
US20170021334A1 (en) | 2017-01-26 |
US9808787B2 (en) | 2017-11-07 |
JP6473162B2 (ja) | 2019-02-20 |
EP3026066A1 (en) | 2016-06-01 |
EP3026066A4 (en) | 2017-01-25 |
DE202014011209U1 (de) | 2018-08-20 |
CN105636990B (zh) | 2018-02-23 |
US20160030921A1 (en) | 2016-02-04 |
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