JPWO2018097324A1 - 繊維と無機粒子の複合体の製造方法、および、繊維と無機粒子の複合体を含有する積層体 - Google Patents
繊維と無機粒子の複合体の製造方法、および、繊維と無機粒子の複合体を含有する積層体 Download PDFInfo
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Abstract
Description
・繊維を含む溶液において無機粒子を合成し、無機粒子と繊維との複合体を製造する工程、無機粒子と繊維との複合体を加工する工程、を含む、無機粒子と繊維との複合体の製造方法。
・無機粒子と繊維との複合体を含有する層と、顔料と接着剤を含有する塗工層、または、接着剤を含有する塗工層と、を含む積層体。
・無機粒子と繊維との複合体を含有する層と、ラミネート層と、を含む積層体。
・無機粒子と繊維との複合体を含有する層と、印刷層と、を含む積層体。
・無機粒子と繊維との複合体を含有する層と、セルロース系繊維と合成繊維とを含む不織布を含有する層と、を含む積層体。
本発明の一態様において、繊維を含む溶液において無機粒子を合成し、無機粒子と繊維との複合体を製造する工程の後に、無機粒子と繊維との複合体を加工する工程を設ける。
本発明の一態様において、繊維を含む溶液において無機粒子を合成し、無機粒子と繊維との複合体を製造する工程の後に、無機粒子と繊維との複合体を塗工する工程を設けることができる。
本発明の一態様においては公知の顔料を用いることができる。その例としては、カオリン、クレー、エンジニアードカオリン、デラミネーテッドクレー、重質炭酸カルシウム、軽質炭酸カルシウム、タルク、二酸化チタン、硫酸バリウム、硫酸カルシウム、酸化亜鉛、珪酸、珪酸塩、コロイダルシリカ、サチンホワイトなどの無機顔料および密実型、中空型、またはコアーシェル型などの有機顔料が挙げられる。これらの顔料は複数種を組合せて使用してもよい。
また、本発明の一態様においては、表面強度向上、耐水性付与および印刷適性筆記適性のうち少なくとも一つを付与するために、澱粉を含有する表面処理液を無機粒子と繊維との複合体に塗工することができる。
得られた無機粒子と繊維との複合体に顔料と接着剤を含む顔料塗工液、または、接着剤を含有する表面処理液を塗工する前に、各種カレンダー装置により原紙に平滑化処理を施すことが好ましい。かかるカレンダー装置としては、スーパーカレンダー、ソフトカレンダー等の一般に使用されているカレンダー装置が適宜使用できる。カレンダー仕上げ条件としては、剛性ロールの温度、カレンダー圧力、ニップ数、ロール速度、カレンダー前の紙水分等が、要求される品質に応じて適宜選択される。
本発明の一態様における顔料と接着剤を含む顔料塗工液は、顔料、接着剤、および必要に応じて添加剤を水に分散または溶解することで調製できる。また、接着剤を含有する表面処理液は、接着剤、および必要に応じて添加剤を水に分散または溶解することで調製できる。前述顔料塗工層を形成できるように各成分の配合は調整される。ブレード塗工を行う場合は、顔料塗工液の固形分濃度は40〜70重量%が好ましく、より好ましくは60〜70重量%である。顔料塗工液の粘度は室温にて60rpmで測定したB型粘度が500〜3000mPa・sの範囲であることが好ましい。
本発明の一態様における塗工する工程は公知の方法で行うことができ、2ロールサイズプレス、ゲートロールコーター、ロットメタリングサイズプレスや、ブレードコーター、スプレーコーター、カーテンコーター等の公知の塗工機を用いることができる。塗工速度も特に限定されないが、ブレードコーターの場合は400〜1800m/分、ロールコーターの場合は400〜2000m/分が好ましい。
湿潤状態の塗工層を乾燥させる方法は限定されず、例えば蒸気加熱シリンダ、加熱熱風エアドライヤ、ガスヒータードライヤ、電気ヒータードライヤ、赤外線ヒータードライヤ等を用いることができる。
本発明の一態様において、繊維を含む溶液において無機粒子を合成し、無機粒子と繊維との複合体を製造する工程の後に、無機粒子と繊維との複合体にラミネートする工程を設けることができる。
本発明の一態様において、繊維を含む溶液において無機粒子を合成し、無機粒子と繊維との複合体を製造する工程の後に、無機粒子と繊維との複合体に印刷する工程を設けることができる。無機粒子と繊維との複合体に印刷することにより、無機粒子と繊維との複合体を含有する層と、印刷層と、を含む積層体が得られる。
本発明の一態様において、繊維を含む溶液において無機粒子を合成し、無機粒子と繊維との複合体を製造する工程の後に、無機粒子と繊維との複合体と同じ材料で作製された複合体との、または別の材料との貼り合わせ工程を設けることができる。
本発明の一態様において、不織布は、セルロース系繊維を含有する。セルロース系繊維は、例えば、木材パルプ;竹、綿、麻、ジュート、ケナフ、農地残廃物、動物(例えばホヤ類)、藻類、微生物(例えば酢酸菌(アセトバクター))生産物などの非木材パルプ;を例示できる。セルロース系繊維としては木材パルプが好ましく、1種又は2種類以上の一般セルロース系繊維を混合して使用することができる。
本発明の一態様において、不織布は、合成繊維、すなわち石油等の有機低分子を重合した合成樹脂からなる繊維を少なくとも一種類以上含む。一般に、合成繊維は、上述のセルロ−ス系繊維に比べ、吸湿性、吸水性、柔軟性等の点では劣るが、寸法安定性、耐光性等の点では優れている。
本発明の一態様において、不織布は、セルロース系繊維、及び合成繊維以外に、必要に応じて、他の材料を一種類以上含んでもよい。他の材料の種類としては、特に限定されないが、例えば、耐熱安定剤、耐候安定剤等の安定剤、充填剤、帯電防止剤、スリップ剤、アンチブロッキング剤、防曇剤、滑剤、染料、顔料、天然油、合成油、ワックス等が挙げられる。これらは一種を用いてもよく、二種以上を併用してもよい。これらの材料の合計含有量は、不織布に対し10質量%を超えない範囲であることが好ましい。
本発明の一態様において、不織布は、上記セルロース系繊維、合成繊維、及び必要に応じて含有される他の材料から、フリースと呼ばれる繊維の集積層を形成し、該繊維同士を結合させ、必要に応じ染色、ラミネート、コーティング等の加工を行うことにより製造することができる。
本発明の一態様においては、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、繊維であれば特に制限されないが、例えば、天然の繊維はもちろん、レーヨンやリヨセルなどの再生繊維(半合成繊維)や合成繊維などを制限なく使用することができる。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)、セルロースナノファイバー、バクテリアセルロース、ホヤなどの動物由来セルロース、藻類が例示され、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。
本発明の一態様において、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。
本発明の一態様において、複合体は、繊維の存在下で無機粒子を合成することによって得ることができる。繊維表面が、無機粒子の析出における好適な場となるため、無機粒子と繊維との複合体を合成しやすいためである。
本発明は、繊維と無機粒子の複合体を含み、水性懸濁液、パルプ、シート、粉体、顆粒、微小球形粒、ペレット、モールド、または、発泡体の形態にして用いる。
本発明の一態様によって得られた複合体は、種々の用途に用いることができ、例えば、紙、繊維、セルロース系複合材料、フィルター材料、塗料、プラスチックやその他の樹脂、ゴム、エラストマー、セラミック、ガラス、タイヤ、建築材料(アスファルト、アスベスト、セメント、ボード、コンクリート、れんが、タイル、合板、繊維板など)、各種担体(触媒担体、医薬担体、農薬担体、微生物担体など)、吸着剤(不純物除去、消臭、除湿など)、しわ防止剤、粘土、研磨材、改質剤、補修材、断熱材、防湿材、撥水材、耐水材、遮光材、シーラント、シールド材、防虫剤、接着剤、インキ、化粧料、医用材料、ペースト材料、変色防止剤、食品添加剤、錠剤賦形剤、分散剤、保形剤、保水剤、濾過助材、精油材、油処理剤、油改質剤、電波吸収材、絶縁材、遮音材、防振材、半導体封止材、放射線遮断材、化粧品、肥料、飼料、香料、塗料・接着剤用添加剤、難燃材料、衛生用品(使い捨ておむつ、生理用ナプキン、失禁者用パッド、母乳パッドなど)等のあらゆる用途に広く使用することができる。また、前記用途における各種充填剤、コーティング剤などに用いることができる。本発明の複合体は、製紙用途に適用してもよく、例えば、印刷用紙、新聞紙、インクジェット用紙、PPC用紙、クラフト紙、上質紙、コート紙、微塗工紙、包装紙、薄葉紙、色上質紙、キャストコート紙、ノンカーボン紙、ラベル用紙、感熱紙、各種ファンシーペーパー、水溶紙、剥離紙、工程紙、壁紙用原紙、不燃紙、難燃紙、積層板原紙、プリンテッドエレクトロニクス用紙、バッテリー用セパレータ、クッション紙、トレーシングペーパー、含浸紙、ODP用紙、建材用紙、化粧材用紙、封筒用紙、テープ用紙、熱交換用紙、化繊紙、減菌紙、耐水紙、耐油紙、耐熱紙、光触媒紙、化粧紙(脂取り紙など)、各種衛生紙(トイレットペーパー、ティッシュペーパー、ワイパー、おむつ、生理用品等)、たばこ用紙、板紙(ライナー、中芯原紙、白板紙など)、紙皿原紙、カップ原紙、ベーキング用紙、研磨紙、合成紙などが挙げられる。すなわち、本発明によれば、一次粒子径が小さくかつ粒度分布の狭い無機粒子と繊維との複合体を得ることができるため、1μm超の粒子径を有していた従来の無機填料とは異なった特性を発揮させることができる。更には、単に無機粒子を繊維に単に配合した場合と異なり、無機粒子を繊維と複合体化しておくと、無機粒子がシートに歩留易いだけでなく、凝集せずに均一に分散したシートを得ることができる。本発明における無機粒子は、好ましい態様において、繊維の外表面・ルーメンの内側に定着するだけでなく、ミクロフィブリルの内側にも生成することが電子顕微鏡観察の結果から明らかとなっている。
以上のように、本発明の一態様は以下の発明を含む。
水酸化マグネシウム140g(和光純薬)と広葉樹晒クラフトパルプ140g(LBKP、CSF:370ml、平均繊維長:0.75mm)を含む水性懸濁液を準備した。この水性懸濁液14Lを、図1に示す45L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体を合成した。反応温度は約36℃、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4L/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続け、炭酸マグネシウム微粒子と繊維との複合体(スラリー中における複合体の濃度:4重量%)を得た。また、得られた複合体の繊維:無機粒子の重量比は、45:55であった。ここで、重量比は、複合体を525℃で約2時間加熱した後、残った灰の重量と元の固形分との比率から求めた灰分に基づいて算出した(JIS P 8251:2003)。
反応容器に3Lのステンレス製容器を用い、パルプの仕込み量を20g、炭酸ガスの吹き込み量を0.57L/minとし、炭酸化反応を35℃のウォーターバス中でスリーワンモーターで撹拌(800rpm)しながら行った以外は、実施例1と同様にして積層体を作製した。なお、得られた複合体の繊維:無機粒子の重量比は、45:55であった。
表面処理液の代わりに、以下の方法により調製した顔料塗工液を用いた以外は、実施例1と同様にして積層体を作製した。
炭酸マグネシウム微粒子と繊維との複合体の代わりに、以下のように合成した硫酸バリウム粒子と繊維との複合体を用いた以外は、実施例3と同様にして積層体を作製した。
繊維分として0.8重量%のアラミド繊維(トワロンRD−1094、帝人、625g)のスラリーを用いた他は、実施例4と同様にして積層体を作製した。なお、得られた複合体の繊維:無機粒子の重量比は55:45であった。
塗工層の代わりに、以下の方法でラミネート層を設けた用いた以外は、実施例1と同様にした。
塗工層の代わりに、以下の方法で印刷層を設けた用いた以外は、実施例1と同様にして積層体を作製した。
塗工層の代わりに、以下の方法で製造する不織布を含有する層を複合体シートに貼り付けた以外は、実施例1と同様にして積層体を作製した。
炭酸マグネシウムと繊維との複合体の代わりに、以下の方法で合成したハイドロタルサイトと繊維との複合体用いた以外は、実施例7と同様にして積層体を作製した。
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、MgCl2(和光純薬)およびAlCl3(和光純薬)の混合水溶液、ZnCl2(和光純薬)およびAlCl3(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:0.05M、NaOH濃度:0.8M)
・酸溶液(B溶液、Mg系、MgCl2濃度:0.3M、AlCl3濃度:0.1M)
・酸溶液(B溶液、Zn系、ZnCl2濃度:0.3M、AlCl3濃度:0.1M)
(2)複合体の合成
アルカリ溶液を10L容の反応容器に入れ、撹拌しながら酸溶液(Mg系)を滴下してハイドロタルサイト微粒子(Mg6Al2(OH)16CO3・4H2O)を合成した。反応温度は60℃、滴下速度は15ml/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、約10倍量の水を用いて水洗して塩を除去した。
塗工層の代わりに、以下の方法で炭酸マグネシウム粒子と繊維との複合体同士を貼り合わせたものを用いた以外は、実施例1と同様にして積層体を作製した。
表面処理液を含有する塗工層を設けなかった以外は、実施例1と同様にして炭酸マグネシウム粒子と繊維との複合体シートを作成した。
それぞれ下記の評価手順に基づいて評価した。
・坪量:JIS P 8124:1998
・灰分:JIS P 8251:2003
・表面強度及び印刷適性:
RI印刷試験機(4色機、石川島産業機械株式会社製)を用い、SMXインキ(タック
グレード20、東洋インキ製造株式会社製)を使用して、インキ盛量7ccで印刷した際
の、ドライピックを調べた。具体的には、印刷後の紙むけ状態を肉眼で観察し、3段階(
優:3>2>1:劣)で評価し、紙むけが少ないほど高評価とした。
・耐水性:RI印刷試験機(4色機、石川島産業機械株式会社製)を用い、SMXインキ(タックグレード20、東洋インキ製造株式会社製)を使用して、インキ盛量7ccで印刷した。印刷サンプルを温水(水道水、40℃)にどぶ漬けし、24時間後に水中から取り出して風乾した。風乾後のサンプルの印字部を肉眼で観察し、3段階(優:3>2>1:劣)で評価した。
・美麗性:RI印刷試験機(4色機、石川島産業機械株式会社製)を用い、SMXインキ(タックグレード20、東洋インキ製造株式会社製)を使用して、インキ盛量7ccで印刷した。印刷サンプルの印字部を肉眼で観察し、3段階(優:3>2>1:劣)で評価した。
・耐久性:サンプルに対し、高さ1mから100gの球を落下させたときに、サンプル表面に破れが生じた場合は(1不合格)、破れが生じない場合は(3合格)とした。
Claims (12)
- 繊維を含む溶液において無機粒子を合成し、無機粒子と繊維との複合体を製造する工程、
無機粒子と繊維との複合体を加工する工程、
を含む、無機粒子と繊維との複合体の製造方法。 - 前記無機粒子と繊維との複合体を加工する工程がシート化する工程である、
請求項1に記載の製造方法。 - 無機粒子と繊維との複合体をシート化する工程を前記加工する工程の前にさらに含む、
請求項1に記載の製造方法。 - 前記無機粒子と繊維との複合体を加工する工程が塗工工程である、
請求項1〜3のいずれか1項に記載の製造方法。 - 前記無機粒子と繊維との複合体を加工する工程がラミネート工程である、
請求項1〜3のいずれか1項に記載の製造方法。 - 前記無機粒子と繊維との複合体を加工する工程が印刷工程である、
請求項1〜3のいずれか1項に記載の製造方法。 - 前記無機粒子と繊維との複合体を加工する工程が当該複合体と同じ材料、または、当該複合体とは別の材料との貼り合わせ工程である、
請求項1〜3のいずれか1項に記載の製造方法。 - 前記別の材料が不織布である、請求項7に記載の製造方法。
- 無機粒子と繊維との複合体を含有する層と、
顔料と接着剤を含有する塗工層、または、接着剤を含有する塗工層と、
を含む積層体。 - 無機粒子と繊維との複合体を含有する層と、
ラミネート層と、
を含む積層体。 - 無機粒子と繊維との複合体を含有する層と、
印刷層と、
を含む積層体。 - 無機粒子と繊維との複合体を含有する層と、
セルロース系繊維と合成繊維とを含む不織布を含有する層と、
を含む積層体。
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Publication number | Publication date |
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EP3546641A1 (en) | 2019-10-02 |
EP3546641B1 (en) | 2023-01-25 |
EP3546641A4 (en) | 2019-10-02 |
US20190368121A1 (en) | 2019-12-05 |
JP7034936B2 (ja) | 2022-03-14 |
WO2018097324A1 (ja) | 2018-05-31 |
CN110214209A (zh) | 2019-09-06 |
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