JP2016532020A - 表面修飾セルロースナノ繊維、バイオ複合樹脂組成物およびその製造方法 - Google Patents
表面修飾セルロースナノ繊維、バイオ複合樹脂組成物およびその製造方法 Download PDFInfo
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Abstract
Description
置換度としての「DS」、
ポリビニルアルコールとしての「PVOH」および「PVA」、
ナノ繊維化セルロースとしての「NFC」。
・ セルロース繊維をアリル化する工程、
・ アリル化セルロース繊維をエポキシ化し、エポキシ-セルロース分散液(単数または複数)を生成する工程、
・ エポキシ-セルロース分散液(単数または複数)を熱可塑性(PVOH)樹脂溶液(単数または複数)に添加する工程、
・ アリル化およびエポキシ化したセルロース群と熱可塑性樹脂(単数または複数)とを、加熱により、もしくは触媒により、または両方により架橋し、反応分散液を得る工程、並びに
・ 前工程で得られた反応分散液を加熱および混合する工程
を有し、セルロース繊維を解繊する工程をさらに含む。
セルロース原料は、漂白したカバノキまたはマツのクラフトから得られたパルプを含んでいた。漂白したカバノキまたはマツのクラフトから得られたこのセルロース繊維10gを、水分含量が最大50%になるまで乾燥させた。パルプのセルロース繊維を、アリルグリシジルエーテルを(0.4〜1.2モル/AGUの量で)添加することによりアリル化し、水4.0 mlに溶解したNaOH 0.4gを含む溶液と混合させ、続いて得られた混合液を繊維と十分に混合させ、45℃で16時間、混合液を攪拌した。得られたアリル化繊維(下記の表2に示されるように、0.2のDS(アリル)を有する)を、その後水で濾過洗浄した。
エポキシ-NFCを最初に調製し、繊維を精錬し、その後複合樹脂組成物を別に調製するのではなく、エポキシセルロース繊維を、反応性精錬を用いて、熱可塑性樹脂懸濁液中で直接精錬した。修飾-NFC-エポキシのエポキシ基を、1,6-ジアミノヘキサン(エポキシ-NFC量の2重量%)を使用し、そして懸濁液を80℃で2時間、激しく撹拌しながら加熱することにより再活性化した。
実施例1で調製したエポキシ-NFC水性分散液の異なる量を、水性熱可塑性樹脂溶液に添加した。ポリマーがセルロース網に浸透するように、混合液を一晩激しく撹拌した。修飾-NFC-エポキシ基と熱可塑性樹脂との間の架橋反応を、過酸化水素を用いることおよび反応分散液を30℃の温度にまで加熱することにより、または実施例2に記載の反応性精錬を利用することにより開始した。
Claims (21)
- アスペクト比が20〜300であり、平均直径が3nm〜100nmであることを特徴とし、ヒドロキシル基が少なくとも1つの修飾基で化学的に修飾されている、セルロースナノ繊維。
- 前記少なくとも1つの修飾基が、アリル基もしくはエポキシ基、または両方を含むことを特徴とする、請求項1に記載のセルロースナノ繊維。
- 平均合計置換度が0.02〜0.7であることを特徴とする、請求項1または2のいずれか一項に記載のセルロースナノ繊維。
- ヒドロキシル基全体の0.01%〜60%が化学的に修飾されていることを特徴とする、請求項1〜3のいずれか一項に記載のセルロースナノ繊維。
- 請求項1〜4のいずれか一項に記載のセルロースナノ繊維を、少なくとも1つの生分解性樹脂に含む、バイオ複合樹脂組成物。
- 少なくとも1つの樹脂が熱可塑性樹脂であり、好ましくはポリビニルアルコール(PVOH)である、請求項5に記載のバイオ複合樹脂組成物。
- 前記組成物が、複合原料全体の0.5重量%〜1.5重量%のセルロース原料を含むことを特徴とする、請求項5または6のいずれか一項に記載のバイオ複合樹脂組成物。
- 請求項5〜7のいずれか一項に記載のバイオ複合樹脂組成物から、該バイオ複合樹脂組成物を周囲温度で鋳造し、乾燥させることにより製造されていることを特徴とする、セルロースナノ繊維強化複合体。
- 厚さが100μm〜300μm、好ましくは200μm未満、特に100μmであることを特徴とする、請求項8に記載のセルロースナノ繊維強化複合体。
- 厚さが100μmであり、500nmの波長における平均光透過率が少なくとも75%、好ましくは85%より大きいことを特徴とする、請求項8または9のいずれか一項に記載のセルロースナノ繊維強化複合体。
- 縦弾性係数が少なくとも2.0GPa、好ましくは3.5GPaであり、引張強さが少なくとも50MPa、好ましくは90 MPaであり、破断時引張歪みが少なくとも180%であることを特徴とする、請求項8〜10のいずれか一項に記載のセルロースナノ繊維強化複合体。
- セルロース原料が、解繊されてナノ繊維(NFC繊維)を生成し、かつ、少なくとも乾燥修飾工程を使用して化学的に修飾されることを特徴とし、該解繊が該化学修飾の前または後に行われる、化学的に修飾されたセルロースナノ繊維を製造するための方法。
- 前記セルロースナノ繊維がアリル化され、その後にエポキシ化工程が好ましくは行われることを特徴とする、請求項12に記載の方法。
- バイオ複合樹脂組成物の製造方法であって、以下の工程:
a)セルロース繊維をアリル化する工程、
b)該アリル化セルロース繊維をエポキシ化し、少なくとも1つのエポキシ-セルロース分散液を生成する工程、
c)該少なくとも1つのエポキシ-セルロース分散液を少なくとも1つの熱可塑性(PVOH)樹脂溶液に添加する工程、
d)アリル化およびエポキシ化したセルロース群と少なくとも1つの熱可塑性樹脂とを、加熱により、もしくは触媒により、または両方により架橋し、反応分散液を得る工程、並びに
e)工程d)で得られた反応分散液を加熱および混合する工程
を有することを特徴とし、
該セルロース繊維が、工程a)の前に、または場合により工程b)の後に、好ましくは工程a)の前に解繊され、セルロースナノ繊維(NFC繊維)を得る方法。 - 前記セルロース繊維が、前処理されていないカバノキまたはマツのセルロースクラフトパルプから得られることを特徴とする、請求項12〜14のいずれか一項に記載の方法。
- 前記アリル化が、アリルグリシジルエーテルを用いて行われることを特徴とする、請求項13〜15のいずれか一項に記載の方法。
- 前記エポキシ化が、水性炭酸ナトリウム/重炭酸ナトリウム緩衝溶液を用いて行われることを特徴とする、請求項13〜16のいずれか一項に記載の方法。
- 前記架橋が、前記混合物を好ましくは30℃の温度にまで加熱し、過酸化水素との反応を開始することにより活性化されることを特徴とする、請求項14〜17のいずれか一項に記載の方法。
- c)〜e)の工程が、1,6-ジアミノヘキサンを用い、熱可塑性樹脂で前記エポキシ-セルロース繊維を直接精錬する反応性精錬の工程と、該懸濁液を、好ましくは80℃の温度にまで加熱する工程とに置き換えられることを特徴とする、請求項14〜18のいずれか一項に記載の方法。
- 前記セルロース繊維が機械的せん断により解繊され、アスペクト比が20〜300、および平均直径が3nm〜100nmとなることを特徴とする、請求項12〜19のいずれか一項に記載の方法。
- 請求項1〜4に記載のセルロースナノ繊維、請求項5〜7に記載のバイオ複合樹脂組成物、請求項8〜11に記載のセルロースナノ繊維強化複合体、または生分解性NFC-PVOH複合材料を製造するための請求項14〜20に記載のバイオ複合樹脂組成物の製造方法の使用。
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JP6419276B1 (ja) * | 2016-12-28 | 2018-11-07 | 旭化成株式会社 | セルロース含有樹脂組成物 |
JPWO2018008736A1 (ja) * | 2016-07-08 | 2019-04-25 | 王子ホールディングス株式会社 | シート |
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WO2015033026A1 (en) | 2015-03-12 |
CN106414505B (zh) | 2020-08-11 |
CN106414505A (zh) | 2017-02-15 |
US10266688B2 (en) | 2019-04-23 |
EP3041870A1 (en) | 2016-07-13 |
EP3041870A4 (en) | 2017-04-26 |
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