JP7269454B1 - 複合繊維を含有する組成物およびその製造方法 - Google Patents
複合繊維を含有する組成物およびその製造方法 Download PDFInfo
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- JP7269454B1 JP7269454B1 JP2022575328A JP2022575328A JP7269454B1 JP 7269454 B1 JP7269454 B1 JP 7269454B1 JP 2022575328 A JP2022575328 A JP 2022575328A JP 2022575328 A JP2022575328 A JP 2022575328A JP 7269454 B1 JP7269454 B1 JP 7269454B1
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- 125000000297 undecanoyl group Chemical group O=C([*])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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Abstract
Description
[1] 無機粒子がセルロース繊維に定着している複合繊維と、熱可塑性樹脂と、を含有する組成物であって、複合繊維のセルロース繊維表面の15%以上が無機粒子によって被覆されており、複合繊維と熱可塑性樹脂を97:3~50:50の重量比で含有する、上記組成物。
[2] 前記セルロース繊維が広葉樹晒クラフトパルプ(LBKP)と針葉樹晒クラフトパルプ(NBKP)を含み、LBKP/NBKPとの重量比が50/50~5/95である、[1]に記載の組成物。
[3] 前記熱可塑性樹脂が、ポリエステル樹脂および/またはポリ乳酸樹脂を含む、[1]または[2]に記載の組成物。
[4] 前記無機粒子が、炭酸マグネシウム、硫酸バリウム、水酸化アルミニウムおよびハイドロタルサイトからなる群より選択される、[1]~[3]のいずれかに記載の組成物。
[5] 前記複合繊維の固形分濃度0.1%の水性懸濁液を60メッシュ(目開き250μm)の篩で濾過処理したとき、処理前の複合繊維の無機物量(A)に対する濾過後に篩上に残る残渣の無機物量(B)の重量割合であるB/Aが50%以上である、[1]~[4]のいずれかに記載の組成物。
[6] [1]~[5]のいずれかに記載の組成物を含む製品。
[7] [1]~[5]のいずれかに記載の組成物を含むシート。
[8] 前記シートの坪量が100g/m2以上であり、厚さが100μm以上である、[7]に記載のシート。
[9] [1]~[5]のいずれかに記載の組成物を製造する方法であって、無機粒子がセルロース繊維に定着している複合繊維を、熱可塑性樹脂と混合することと、前記複合繊維と前記熱可塑性樹脂との混合物を加熱処理することと、を含む、上記方法。
本発明において、繊維と複合化する無機粒子は特に制限されないが、水に不溶性または難溶性の無機粒子であることが好ましい。無機粒子の合成を水系で行う場合があり、また、複合体を水系で使用することもあるため、無機粒子が水に不溶性または難溶性であると好ましい。
本発明で使用する複合体の一例として、ハイドロタルサイト(HT)と繊維との複合体について以下に説明する。本複合体は高い消臭特性を有する。
本発明においては、繊維の存在下で溶液中においてハイドロタルサイトを合成することによって、ハイドロタルサイトと繊維の複合体を製造する。
本発明において合成反応の温度は、例えば、30~100℃とすることができるが、40~80℃が好ましく、50~70℃がより好ましく、60℃程度とすると特に好ましい。温度が高すぎたり低すぎたりすると、反応効率が低下しコストが高くなる傾向がある。
本発明においては、無機粒子と繊維とを複合体化する。複合体を構成する繊維は、セルロース繊維であれば特に制限されない。セルロース繊維の原料としては、パルプ繊維(木材パルプや非木材パルプ)、バクテリアセルロースが例示され、木材パルプは、木材原料をパルプ化して製造すればよい。木材原料としては、アカマツ、クロマツ、トドマツ、エゾマツ、ベニマツ、カラマツ、モミ、ツガ、スギ、ヒノキ、カラマツ、シラベ、トウヒ、ヒバ、ダグラスファー、ヘムロック、ホワイトファー、スプルース、バルサムファー、シーダ、パイン、メルクシマツ、ラジアータパイン等の針葉樹、及びこれらの混合材、ブナ、カバ、ハンノキ、ナラ、タブ、シイ、シラカバ、ハコヤナギ、ポプラ、タモ、ドロヤナギ、ユーカリ、マングローブ、ラワン、アカシア等の広葉樹及びこれらの混合材が例示される。
本発明においては、上記の複合繊維に加えて熱可塑性繊維を使用する。本発明において使用する熱可塑性繊維は、複合体(複合繊維)との混合性や抄紙性(搾水性、地合)の観点からして、ポリエステル系、ポリプロピレン系、ポリエチレン系の合成繊維を用いることが好適である。特に、混合性を考慮する場合は、ポリエステル系の合成繊維を使用することが好ましい。
本発明に係る組成物は、上述した成分以外のものを含んでもよい。例えば、湿潤紙力剤(紙力増強剤)を添加して湿潤強度を向上させることができる。湿潤紙力剤としては、例えば、尿素ホルムアルデヒド樹脂、メラミンホルムアルデヒド樹脂、ポリアミド・ポリアミン・エピクロロヒドリン樹脂、植物性ガム、ラテックス、ポリエチレンイミン、グリオキサール、ガム、マンノガラクタンポリエチレンイミン樹脂、ポリアクリルアミド樹脂、ポリビニルアミン樹脂、ポリビニルアルコール等の樹脂;前記樹脂から選ばれる2種以上からなる複合ポリマー又は共重合ポリマー;澱粉及び加工澱粉;カルボキシメチルセルロース、グアーガム、尿素樹脂等が挙げられる。湿潤紙力剤を複合体にさらに加える場合には、複合体を製造した後に得られるスラリーに、さらに湿潤紙力剤を添加して、その後抄紙すればよい。湿潤紙力剤の含有量は、用途に応じて適宜に調整することができるが、その効果をより好適に発揮させるためには、例えば、複合体の重量に対して0.1~1.0重量%とすることが好ましく、0.3~0.7重量%とすることがさらに好ましい。
1-1.複合繊維の合成
(1)複合繊維1:炭酸マグネシウムとセルロース繊維との複合繊維
水酸化マグネシウム5250g(宇部マテリアルズ、UD653)とクラフトパルプ3500g(LBKP/NBKP=50/50、CSF=360mL、平均繊維長=0.76mm)を含む水性懸濁液170Lを準備した。これを500L容のキャビテーション装置に入れ、反応溶液を循環させながら、反応容器中に炭酸ガスを吹き込んで炭酸ガス法によって炭酸マグネシウム微粒子と繊維との複合繊維を合成した。反応温度は約40℃、炭酸ガスは市販の液化ガスを供給源とし、炭酸ガスの吹き込み量は20L/minとした。反応液のpHが約7.8になった段階でCO2の導入を停止し(反応前のpHは約9.5)、その後30分間、キャビテーションの発生と装置内でのスラリーの循環を継続してサンプルを得た(図1)。
まず、ハイドロタルサイト(HT)を合成するための溶液を準備した。アルカリ溶液(A溶液)として、Na2CO3(和光純薬)およびNaOH(和光純薬)の混合水溶液を調製した。また、酸溶液(B溶液)として、MgSO4(和光純薬)およびAl2(SO4)3(和光純薬)の混合水溶液を調製した。
・アルカリ溶液(A溶液):Na2CO3濃度:0.1M、NaOH濃度:1.6M
・酸溶液(B溶液):MgSO4濃度:0.6M、Al2(SO4)3濃度:0.1M
次いで、アルカリ溶液(A溶液)にパルプ繊維(LBKP/NBKP=50/50)を添加し、パルプ繊維を含む水性懸濁液を準備した(パルプ固形分30g、パルプ繊維濃度:1.56%、pH:約12.4)。この水性懸濁液を10L容の反応容器に入れ、水性懸濁液を撹拌しながら、酸溶液(B溶液)を滴下してハイドロタルサイト粒子と繊維との複合繊維を合成した(A液の量:1.1L、B液の量:1.1L)。反応温度は60℃、滴下速度は5ml/minであり、反応液のpHが約7になった段階で滴下を停止した。滴下終了後、30分間、反応液を撹拌し、10倍量の水を用いて水洗して塩を除去した(図2)。
水酸化アルミニウムを合成するための溶液を準備した。アルカリ溶液として、NaOH(和光純薬 製)水溶液(A溶液)を調製した。また、酸溶液として、市販の硫酸アルミニウム水溶液(硫酸バンド、朝日化学工業製)をそのまま使用した。
・アルカリ溶液(A溶液、水酸化ナトリウム濃度:25%)
・酸溶液(B溶液、硫酸アルミニウム濃度:約27%)
(1)繊維と無機粒子の重量比
複合繊維のスラリー(固形分換算で3g)について、ろ紙を用いて吸引濾過した後、残渣をオーブンで乾燥し(105℃、2時間)、JIS P 8251:2003に基づいて灰分を測定し、複合繊維の繊維:無機粒子の重量比を算出した。ただし、525℃での灰化処理によって重量減少が生じるため、灰化処理後の実測重量から重量減少分を踏まえて算出した。
複合繊維サンプルをそれぞれエタノールで洗浄後、電子顕微鏡(SEM)によって観察して、無機粒子による繊維表面の被覆率を評価した。電子顕微鏡観察の結果から、無機粒子の一次粒子径を計測した。
濾過処理前のサンプルの無機物量(A)と濾過後に篩上に残る残渣の無機物量(B)を測定し、下記の式により、濾過処理を経ても繊維に定着している無機分率(B/A)を算出した。
・濾過処理前の複合繊維の無機物量(A): 複合繊維スラリー(固形分換算で3g)を濾紙で吸引濾過した後、残渣をオーブンで乾燥し(105℃、2時間)、灰分を測定することによって測定した。
・濾過後に篩上に残る残渣の無機物量(B): 複合体サンプル(固形分換算で1g)を固形分濃度が0.1%となるように水で希釈し、懸濁液0.2リットルを、60メッシュ(目開き250μm)の篩ですべて濾過し、0.6リットルの水で洗浄した。次いで、濾過後の篩残渣について、灰分を測定して無機粒子の重量比率(B)を測定した。
2-1.手抄きシートの製造
(1)シート1
複合繊維1の水性懸濁液(約1.5%)に、熱可塑性樹脂としてポリエステル繊維(繊維長:5mm)を加えて、複合繊維とポリエステル繊維の重量比が90:10となるように調整した。この水性懸濁液から、JIS P 8222に基づく角形手抄き器にて湿紙を作成し、これを130℃に加熱したステンレス板に挟み、プレス機(熊谷理機製)で1MPa、1分間プレス処理してシートを製造した。
複合繊維1の代わりに複合繊維2を用いた以外は、シート1と同様にシートを製造した。
複合繊維1の代わりに複合繊維3を用いた以外は、シート1と同様にシートを製造した(図4)。
複合繊維3とポリエステル繊維の重量比を50:50となるように調整した以外は、シート3と同様にシートを製造した。
複合繊維3とポリエステル繊維の重量比を97:3となるように調整した以外は、シート3と同様にシートを製造した(図5)。
熱可塑性樹脂として、ポリエステル繊維の代わりにポリ乳酸繊維を用いた以外は、シート3と同様にシートを製造した(図6)。
熱可塑性樹脂を用いない以外は、シート3と同様にシートを製造した。
複合繊維3の代わりにパルプ繊維(LBKP/NBKP=8/2)を用いた以外は、シート3と同様にシートを製造した。
パルプ繊維(LBKP/NBKP=8/2)の水性懸濁液(約1.5%)に、熱可塑性樹脂としてポリエステル繊維(繊維長:5mm)を加えて、パルプ繊維とポリエステル繊維の重量比が90:10となるように調整した。これに水酸化アルミニウム(B-103、日本軽金属)を混合し、アニオン性歩留剤(FA230、ハイモ社製)を200ppm、カチオン性歩留剤(ND300、ハイモ社製)を200ppm添加し、500rpmにて撹拌して懸濁液を調成した。得られた懸濁液から、JIS P 8222に基づく角形手抄き器にて湿紙を作成し、これを130℃に加熱したステンレス板に挟み、プレス機(熊谷理機製)で1MPa、1分間プレス処理してシートを製造した。
得られた手抄きシートの物性について、下記の手順に基づいて評価した。
(1)坪量、厚さ、密度
坪量はJIS P 8124:1998、厚さはJIS P 8118:1998に基づいて評価した。また、密度は、厚さと坪量の測定値より算出した。
JIS P 8251:2003に基づいて測定した。ただし、525℃での灰化処理によって重量減少が生じるため、灰化処理後の実測重量から重量減少分を踏まえて算出した。
23℃、50%RHで調湿したサンプルを、100mm×15mmに切り出して、短辺を2分割する基準線を長軸方向に引き、長さ(L)を測定した。次いで、30℃、90%RHに設定した部屋で24時間サンプルを静置した後、再び基準線の長さ(L´)を測定した。その後、寸法変化率[(L´-L)/L×100、%]を算出し、下記の基準に基づいて評価した。
◎:寸法変化率が0.4%未満
〇:寸法変化率が0.4%以上0.7%未満
△:寸法変化率が0.7%以上1.0%未満
×:寸法変化率が1.0%以上
粉おちを下記の基準に基づいて目視で確認した。まず、サンプルをカッターもしくはハサミで切断し、紙粉発生の有無を目視で確認した。次に、切り出したサンプル片を親指と人差し指で挟むように持ち、机にセットされた黒画用紙の上で、サンプル片が折れ曲がらない程度の軽い力でタッピングした。このとき、サンプル片の切断面が机に対して垂直となるようにして実施した。その後、黒画用紙の上に付着した粉の状態を目視で判定した。
◎:粉おちが極めて少なく、紙粉も発生しない
〇:粉おちが少ない
△:粉おちが生じるが、紙粉は少ない
×:粉おちが多く、紙粉も多く発生する
JIS A 1322(JIS Z 2150)を基にして、以下の手順により難燃性を評価した。
・炭化長:試験体の加熱面の炭化部分(炭化して明らかに強度が変化)している部分について支持枠の長手方向の最大長さを測定する。
・残炎時間:加熱終了時から試験体が炎をあげて燃え続ける時間を測定する。
・残じん:加熱終了時から無炎燃焼している状態をいう。
〇(難燃性あり):加熱終了から1分後に残じんがなく、炭化長15cm以内かつ残炎時間5秒以下
△(やや難燃性):加熱終了から1分後に残じんがあるが、炭化長15cm以内かつ残炎時間5秒以下
×(難燃性なし):加熱終了から1分後に残じんがあり、炭化長15cm超または残炎時間5秒超
Claims (7)
- 無機粒子がセルロース繊維に定着している複合繊維と、熱可塑性樹脂と、を含有する組成物であって、
複合繊維のセルロース繊維表面の15%以上が無機粒子によって被覆されており、複合繊維と熱可塑性樹脂を97:3~50:50の重量比で含有し、無機粒子が、炭酸マグネシウム、硫酸バリウムおよび水酸化アルミニウムからなる群より選択され、熱可塑性樹脂がポリエステル樹脂および/またはポリ乳酸樹脂を含む、上記組成物。 - 前記セルロース繊維が広葉樹晒クラフトパルプ(LBKP)と針葉樹晒クラフトパルプ(NBKP)を含み、LBKP/NBKPとの重量比が、50/50~5/95である、請求項1に記載の組成物。
- 前記複合繊維の固形分濃度0.1%の水性懸濁液を60メッシュ(目開き250μm)の篩で濾過処理したとき、処理前の複合繊維の無機物量(A)に対する濾過後に篩上に残る残渣の無機物量(B)の重量割合であるB/Aが50%以上である、請求項1に記載の組成物。
- 請求項1~3のいずれかに記載の組成物を含む製品。
- 請求項1~3のいずれかに記載の組成物を含むシート。
- 前記シートの坪量が100g/m2以上であり、厚さが100μm以上である、請求項5に記載のシート。
- 請求項1~3のいずれかに記載の組成物を製造する方法であって、
無機粒子がセルロース繊維に定着している複合繊維を熱可塑性樹脂と混合することと、
前記複合繊維と前記熱可塑性樹脂との混合物を加熱処理することと、
を含む、上記方法。
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JPS61258865A (ja) * | 1985-05-13 | 1986-11-17 | Calp Corp | 複合樹脂組成物 |
JP2002138170A (ja) * | 2000-10-31 | 2002-05-14 | Ykk Corp | セルロース系粉体含有複合樹脂成形体及びその製造方法 |
JP2019002004A (ja) * | 2017-06-16 | 2019-01-10 | 凸版印刷株式会社 | 光熱変換材料、光熱変換組成物、および光熱変換成形体 |
WO2019135384A1 (ja) * | 2018-01-05 | 2019-07-11 | 凸版印刷株式会社 | 複合粒子、複合粒子の製造方法、乾燥粉体、および成型用樹脂組成物 |
JP2019137938A (ja) * | 2018-02-09 | 2019-08-22 | 日本製紙株式会社 | 湿式不織布 |
JP2021123840A (ja) * | 2020-01-31 | 2021-08-30 | 日本製紙株式会社 | 抗アレルゲン繊維製品 |
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JPS61258865A (ja) * | 1985-05-13 | 1986-11-17 | Calp Corp | 複合樹脂組成物 |
JP2002138170A (ja) * | 2000-10-31 | 2002-05-14 | Ykk Corp | セルロース系粉体含有複合樹脂成形体及びその製造方法 |
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