JP2018505259A - 相互侵入高分子網目材料の製造方法、その製品、及び当該製品の使用 - Google Patents
相互侵入高分子網目材料の製造方法、その製品、及び当該製品の使用 Download PDFInfo
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- JP2018505259A JP2018505259A JP2017533211A JP2017533211A JP2018505259A JP 2018505259 A JP2018505259 A JP 2018505259A JP 2017533211 A JP2017533211 A JP 2017533211A JP 2017533211 A JP2017533211 A JP 2017533211A JP 2018505259 A JP2018505259 A JP 2018505259A
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- Prior art keywords
- ipn
- trimethylammonium chloride
- ethyl
- mcc
- mfc
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- UZNHKBFIBYXPDV-UHFFFAOYSA-N trimethyl-[3-(2-methylprop-2-enoylamino)propyl]azanium;chloride Chemical compound [Cl-].CC(=C)C(=O)NCCC[N+](C)(C)C UZNHKBFIBYXPDV-UHFFFAOYSA-N 0.000 claims description 7
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Abstract
Description
i)微結晶性セルロース(MCC)、微小繊維状セルロース(MFC)、又はそれらの混合物、及び少なくとも1種のモノマーを含む水性溶液を提供するステップ;
ii)in situで少なくとも1種の上記モノマーを重合し、MCC、MFC又はそれらの混合物とともに、IPNを形成するステップ;及び
iii)IPN材料を得るステップ、を含む、相互侵入高分子網目(IPN)材料の製造方法が提供される。
[2−(アクリロイルオキシ)エチル]トリメチルアンモニウムクロリド、(3−アクリルアミドプロピル)トリメチルアンモニウムクロリド、アクリル酸2−(ジエチルアミノ)−エチル、アクリル酸2−(ジメチルアミノ)−エチル、[2−(メタクリロイルオキシ)エチル]−トリメチルアンモニウムクロリド、[3−(メタクリロイルアミノ)プロピル]トリメチルアンモニウムクロリドからなる群から選ばれるカチオン性モノマー、
アクリル酸、塩化アクリル、メタクリル酸、2−アクリルアミド−2−メチルプロパンスルホン酸、2−(アクリロイルアミノ)−2−メチル−1−プロパンスルホン酸ナトリウムからなる群から選ばれるアニオン性モノマー、
又はそれらの混合物からなる群から選択される。
微結晶性セルロース(MCC)、微小繊維状セルロース(MFC)又はそれらの混合物;及び
MCC、MFC又はそれらの混合物とともに、IPNを形成する少なくとも1種のポリマー
を含む、相互侵入高分子網目(IPN)が提供される。
アクリルアミド、N−メチロールアクリルアミド、N−メチロール(メタ)アクリルアミド、N,N−ジメチルアミノプロピルアクリルアミド、N,N−ジメチルアミノプロピルアクリルアミド、N,N−ジメチル−アミノプロピルメタクリルアミド,N,N−ジメチルアミノエチルアクリルアミド、N−[2−(ジ−メチルアミノ)−1,1−ジメチル−エチル]−アクリルアミド、
[2−(アクリロイルオキシ)エチル]トリメチルアンモニウムクロリド、(3−アクリルアミドプロピル)トリメチルアンモニウムクロリド、アクリル酸2−(ジエチルアミノ)−エチル、アクリル酸2−(ジメチルアミノ)−エチル、[2−(メタクリロイルオキシ)エチル]−トリメチルアンモニウムクロリド、[3−(メタクリロイルアミノ)プロピル]トリメチルアンモニウムクロリドからなる群から選ばれるカチオン性モノマー、
アクリル酸、塩化アクリル、メタクリル酸、2−アクリルアミド−2−メチルプロパンスルホン酸、2−(アクリロイルアミノ)−2−メチル−1−プロパンスルホン酸ナトリウムからなる群から選ばれるアニオン性モノマー、
又はそれらの混合物
からなる群から選択される少なくとも1種のモノマーの重合反応において形成されるポリマー又はコポリマーである。
300gの水の中で、Kemira社製の微結晶性セルロース(MCC) 30%(96.27g)を95℃で、30分の間、溶液が半透明になるまで加熱した。次いで、このセルロース水溶液を冷却し、1Lデュワーフラスコに投入した。モノマーとして、Kemira社製のアクリルアミド50%(448g)、及びKemira社製の[2−(アクリロイルオキシ)エチル]トリメチルアンモニウムクロリド溶液80%(81g)をフラスコに添加し、攪拌した。モノマーの後、アジピン酸(14g)を添加した。フラスコをクリングフィルムで封止して窒素雰囲気を維持し、一定の窒素フローを有する2本の脱気管を挿入した。溶液は、1時間脱気した。アルドリッチ社製の開始剤(V−50及び過硫酸アンモニウム)を添加した。溶液は、濃縮され始めた。窒素のバブリングは、ゲルが形成されるまで続けた。フラスコを3時間放置した。形成されたゲルをフラスコから取り出し、これを小片に切断して、肉挽機に供給した。挽かれたゲルを放置して、乾燥させた。乾燥の後、乾燥されたゲルを製粉し、粉末形態のIPN材料を製造した。
MCCを使用しなかった点以外は、IPN材料と同一の方法で、カチオン性ポリアクリルアミドを作製した。すなわち、カチオン性ポリアクリルアミドを水中で作製し、MCC水性溶液中では作製しなかった。得られた生成物は、粉末状のカチオン性ポリアクリルアミドであった。
調製された、IPN材料、カチオン性ポリアクリルアミド、及びポリアクリルアミドと微結晶性セルロースとの混合物の試料の、粘度、不溶分、及び電荷を測定した。
表1において、カチオン性ポリアクリルアミド(試料HM−0)、本発明のIPN材料(試料HM−MCC−10)、及びポリアクリルアミド及び微結晶性セルロースの混合物(試料HM−0+MCC)の性質を比較する。
濾水性は、異なる用量のHM−0(カチオン性PAM)及びHM−MFC(本発明のIPN材料)で濾水時間を比較することにより検討した。
Claims (20)
- i)微結晶性セルロース(MCC)、微小繊維状セルロース(MFC)、又はそれらの混合物、及び少なくとも1種のモノマーを含む水性溶液を提供するステップ;
ii)in situで少なくとも1種の前記モノマーを重合し、MCC、MFC又はそれらの混合物とともに、IPNを形成するステップ;及び
iii)IPN材料を得るステップ、を含む、相互侵入高分子網目(IPN)材料の製造方法。 - 少なくとも1種の前記モノマーが、カチオン性モノマー又はアニオン性モノマーである、請求項1に記載の製造方法。
- 少なくとも1種の前記モノマーが、
アクリルアミド、N−メチロールアクリルアミド、N−メチロール(メタ)アクリルアミド、N,N−ジメチル−アミノプロピルメタクリルアミド、N,N−ジメチルアミノエチルアクリルアミド、N−[2−(ジ−メチルアミノ)−1,1−ジメチル−エチル]−アクリルアミド、
[2−(アクリロイルオキシ)エチル]トリメチルアンモニウムクロリド、(3−アクリルアミドプロピル)トリメチルアンモニウムクロリド、[2−(メタクリロイルオキシ)エチル]−トリメチルアンモニウムクロリド、[3−(メタクリロイルアミノ)プロピル]トリメチルアンモニウムクロリド、アクリル酸2−(ジエチルアミノ)−エチル、アクリル酸2−(ジメチルアミノ)−エチルからなる群から選ばれるカチオン性モノマー、
アクリル酸、塩化アクリル、メタクリル酸、2−アクリルアミド−2−メチルプロパンスルホン酸、2−(アクリロイルアミノ)−2−メチル−1−プロパンスルホン酸ナトリウムからなる群から選ばれるアニオン性モノマー、
又はそれらの混合物からなる群から選ばれ;
好ましくは、前記モノマーが、アクリルアミド、及び[2−(アクリロイルオキシ)エチル]トリメチルアンモニウムクロリド、(3−アクリルアミドプロピル)トリメチルアンモニウムクロリド、[2−(メタクリロイルオキシ)エチル]−トリメチルアンモニウムクロリド、[3−(メタクリロイルアミノ)プロピル]トリメチルアンモニウムクロリドからなる群から選ばれるカチオン性モノマーであり、
より好ましくは、前記モノマーが、アクリルアミド及び[2−(アクリロイルオキシ)エチル]トリメチルアンモニウムクロリドである、請求項1又は2に記載の製造方法。 - ステップi)における水性溶液のpHが、酸性領域に設定され、好ましくは、2から4の値のpH値に設定され、より好ましくは、アジピン酸を使用して酸性領域に設定される、請求項1から3のいずれかに記載の製造方法。
- ステップii)における重合が、2,2’−アゾビス(2−メチルプロピオンアミジン)2塩酸塩、2,2’−アゾビス[2−(2−イミダゾリン−2−イル)プロパン]2塩酸塩、2,2’−アゾビスイソブチルニトリル(AIBN)、過酸化物、過酸、過硫酸カリウム及び過硫酸アンモニウムのような過硫酸塩、硫酸塩、又はそれらの混合物、好ましくは、過硫酸アンモニウムからなる群から選ばれる1以上の開始剤により開始される、請求項1から4のいずれかの製造方法。
- ステップiii)から得られたIPN材料が乾燥され、好ましくは乾燥されて製粉される、請求項1から5のいずれかに記載の製造方法。
- ステップii)が、不活性雰囲気下、好ましくは、窒素雰囲気下で行われる、請求項1から6のいずれかに記載の製造方法。
- MCC、MFC又はそれらの混合物の量が、IPN材料の量に基づいて、0.5質量%から15質量%、好ましくは1質量%から10質量%、より好ましくは1質量%から5質量%、更により好ましくは1質量%から3質量%、例えば、1.6質量%である、請求項1から7のいずれかに記載の製造方法。
- 微結晶性セルロース(MCC)、微小繊維状セルロース(MFC)、又はそれらの混合物;及び
MCC、MFC又はそれらの混合物とともに、IPNを形成する少なくとも1種のポリマーを含む、相互侵入高分子網目(IPN)材料。 - 少なくとも1種の前記ポリマーが、カチオン性又はアニオン性、好ましくはカチオン性である、請求項9に記載の相互侵入高分子網目(IPN)材料。
- コポリマーが、アクリルアミド、及び[2−(アクリロイルオキシ)エチル]トリメチルアンモニウムクロリド、(3−アクリルアミドプロピル)トリメチルアンモニウムクロリド、[2−(メタクリロイルオキシ)エチル]−トリメチルアンモニウムクロリド、[3−(メタクリロイルアミノ)プロピル]トリメチルアンモニウムクロリド、アクリル酸2−(ジエチルアミノ)−エチル、アクリル酸2−(ジメチルアミノ)−エチルからなる群から選ばれるカチオン性モノマーのコポリマーであり、
好ましくは、アクリルアミド、及び[2−(アクリロイルオキシ)エチル]トリメチルアンモニウムクロリド、(3−アクリルアミドプロピル)トリメチルアンモニウムクロリド、[2−(メタクリロイルオキシ)エチル]−トリメチルアンモニウムクロリド、[3−(メタクリロイルアミノ)プロピル]トリメチルアンモニウムクロリドからなる群から選ばれるカチオン性モノマーのコポリマーであり、
より好ましくは、アクリルアミド及び[2−(アクリロイルオキシ)エチル]トリメチルアンモニウムクロリドのコポリマーである、請求項9又は10に記載の相互侵入高分子網目(IPN)材料。 - IPN材料の電荷密度(Mutek)が、0.5質量%の水性溶液から測定するとき、酸性pHにおいて、1.1meq/gから1.5meq/g、好ましくは1.15meq/gから1.45meq/gである、請求項9から11のいずれかに記載の相互侵入高分子網目(IPN)材料。
- IPN材料の電荷密度(Mutek)が、0.5質量%の水性溶液から測定するとき、中性pHにおいて、0.1meq/gから1.3meq/g、好ましくは0.2meq/gから1.2meq/gである、請求項9から12のいずれかに記載の相互侵入高分子網目(IPN)材料。
- IPN材料が粉末の形態である、請求項9から13のいずれかに記載の相互侵入高分子網目(IPN)材料。
- IPN材料の塩粘度が、60cPから100cP、好ましくは65cPから95cP(0.5質量%水溶液、NaCl 5質量%、18/6スピンドル、30rpm)である、請求項9から14のいずれかに記載の相互侵入高分子網目(IPN)材料。
- MCC、MFC又はそれらの混合物の量が、IPN材料の量に基づいて、0.5質量%から15質量%、好ましくは1質量%から10質量%、より好ましくは1質量%から5質量%、及び更により好ましくは1質量%から3質量%、例えば、1.6質量%である、請求項9から15のいずれかに記載の相互侵入高分子網目(IPN)材料。
- 請求項9から16のいずれかに記載のIPN材料、又は請求項1から8のいずれかに記載の製造方法により製造されるIPN材料の、製紙産業における濾水剤、脱水剤、湿潤紙力増強剤、又は乾燥紙力増強剤としての使用。
- IPN材料の濾水剤としての用量が、乾燥パルプに対して、0.1kg/tonから1kg/ton、好ましくは0.2kg/tonから0.8kg/tonである、請求項17に記載の使用。
- パルプのスラリーを提供するステップと、請求項9から16のいずれかに記載のIPN材料又は請求項1から8のいずれかに記載の製造方法により製造されるIPN材料を前記パルプのスラリーに添加するステップと、金網上でパルプのスラリーを脱水するステップと、脱水されたパルプのスラリーの紙を形成するステップと、を含む、紙又はボードの製造方法。
- 請求項9から16のいずれかに記載のIPN材料、又は請求項1から8のいずれかに記載の製造方法により製造されるIPN材料を、パルプのスラリーに添加することを特徴とする、紙又はボードの製造における濾水を改善する方法。
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CN113248730A (zh) * | 2021-04-22 | 2021-08-13 | 上海健康医学院 | 聚丙烯酰胺-纳米纤维素晶-银纳米颗粒复合导电抗冻有机水凝胶及其制备方法和应用 |
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US10590607B2 (en) | 2020-03-17 |
CA2971528A1 (en) | 2016-06-30 |
EP3237676B1 (en) | 2019-05-15 |
RU2687950C2 (ru) | 2019-05-16 |
KR102482317B1 (ko) | 2022-12-28 |
BR112017013490A2 (pt) | 2018-02-27 |
EP3237676A1 (en) | 2017-11-01 |
FI20146134A (fi) | 2016-06-23 |
CA2971528C (en) | 2023-06-13 |
RU2017121639A3 (ja) | 2019-03-28 |
US20180023253A1 (en) | 2018-01-25 |
AU2015370830A1 (en) | 2017-06-29 |
CN107002364A (zh) | 2017-08-01 |
WO2016102753A1 (en) | 2016-06-30 |
CN107002364B (zh) | 2020-05-15 |
KR20170098295A (ko) | 2017-08-29 |
BR112017013490B1 (pt) | 2022-03-03 |
ES2741825T3 (es) | 2020-02-12 |
JP6834103B2 (ja) | 2021-02-24 |
AU2015370830B2 (en) | 2019-09-12 |
RU2017121639A (ru) | 2019-01-24 |
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