JP5114654B2 - 顔料塗工紙の製造方法 - Google Patents
顔料塗工紙の製造方法 Download PDFInfo
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- JP5114654B2 JP5114654B2 JP2005309514A JP2005309514A JP5114654B2 JP 5114654 B2 JP5114654 B2 JP 5114654B2 JP 2005309514 A JP2005309514 A JP 2005309514A JP 2005309514 A JP2005309514 A JP 2005309514A JP 5114654 B2 JP5114654 B2 JP 5114654B2
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- 230000001186 cumulative effect Effects 0.000 description 1
- OIWOHHBRDFKZNC-UHFFFAOYSA-N cyclohexyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC1CCCCC1 OIWOHHBRDFKZNC-UHFFFAOYSA-N 0.000 description 1
- CPGPQFYAGKHQTB-UHFFFAOYSA-N cyclopentyne Chemical compound C1C[C]=[C]C1 CPGPQFYAGKHQTB-UHFFFAOYSA-N 0.000 description 1
- GTBGXKPAKVYEKJ-UHFFFAOYSA-N decyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCOC(=O)C(C)=C GTBGXKPAKVYEKJ-UHFFFAOYSA-N 0.000 description 1
- FJBFPHVGVWTDIP-UHFFFAOYSA-N dibromomethane Chemical compound BrCBr FJBFPHVGVWTDIP-UHFFFAOYSA-N 0.000 description 1
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- ZWWQRMFIZFPUAA-UHFFFAOYSA-N dimethyl 2-methylidenebutanedioate Chemical compound COC(=O)CC(=C)C(=O)OC ZWWQRMFIZFPUAA-UHFFFAOYSA-N 0.000 description 1
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- 238000012674 dispersion polymerization Methods 0.000 description 1
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- YOZHLACIXDCHPV-UHFFFAOYSA-N n-(methoxymethyl)-2-methylprop-2-enamide Chemical compound COCNC(=O)C(C)=C YOZHLACIXDCHPV-UHFFFAOYSA-N 0.000 description 1
- ULYOZOPEFCQZHH-UHFFFAOYSA-N n-(methoxymethyl)prop-2-enamide Chemical compound COCNC(=O)C=C ULYOZOPEFCQZHH-UHFFFAOYSA-N 0.000 description 1
- LKEDKQWWISEKSW-UHFFFAOYSA-N nonyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCOC(=O)C(C)=C LKEDKQWWISEKSW-UHFFFAOYSA-N 0.000 description 1
- ZWWQICJTBOCQLA-UHFFFAOYSA-N o-propan-2-yl (propan-2-yloxycarbothioyldisulfanyl)methanethioate Chemical compound CC(C)OC(=S)SSC(=S)OC(C)C ZWWQICJTBOCQLA-UHFFFAOYSA-N 0.000 description 1
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- DOIRQSBPFJWKBE-UHFFFAOYSA-N phthalic acid di-n-butyl ester Natural products CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 1
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Description
(1)測定条件:印加圧力:100kPa、加圧時間:30秒、フィルター:0.1μmポアサイズ
(2)W値=(L×r2)/10000
L:加圧脱水量(g/m2)、r:ラテックス平均粒子径(nm)
(3)測定条件:減圧度:700hPa、せん断速度:1(1/s)、初期ギャップ:0.5mm
前記ラテックスの重合に使用されるエチレン系不飽和カルボン酸単量体量が、全モノマー100質量部中3.5質量部以下であることが好ましい。
前記ラテックスの配合量が、顔料全固形分に対して5〜25質量%であることが好ましい。
前記接着剤において、更に澱粉が含有され、澱粉含有量が顔料全固形分に対して0.5〜3質量%以下であることが好ましい。
前記澱粉が、濃度20%、温度40℃にて測定された粘度が30mPa・s以上であることが好ましい。
前記紙基材上に塗工層を設ける方法がブレード塗工方式であることが好ましい。
前記紙基材が、あらかじめ顔料および接着剤を主成分とする下塗り塗工層を少なくとも1層以上設けたものであることが好ましい。
塗工液の不動化時間を、Anton Paar社製レオメーターPhysica MCR101と、同社のイモビリゼーションセルとを組み合わせてなる塗工液の不動化時間を測定する装置を使用して測定した。本装置は、図1に示されるように、レオメーターの測定用パラレルプレート上部11aと下部11bの間に測定対象塗工液17および紙基材19を設置して測定される装置である。イモビリゼーションセルは、パラレルプレート下部11bを含めて下の部分が相当する。パラレルプレート下部11bは鉛直方向に貫通する孔を多数有しており、この孔を介して減圧室13aと空間的に接している。このため、減圧ポンプに接続された接続口13bから減圧することにより減圧室13aは減圧され(本発明の条件としては、700hPa)、紙基材19および測定対象塗工液17も減圧を受けることになる。減圧下においては塗工液中から水が失われるため塗工液の体積は減少し、パラレルプレート間のギャップ、即ち11aの下部と11bの上部との距離(本発明の条件としては、初期ギャップ:0.5mm)は減少するが、これはパラレルプレート上部11aに結合している法線応力検出部および回転速度制御部15で測定される法線応力が、一定範囲にはいるよう自動的にギャップが調整され、さらには塗工液に与えられるせん断速度(本発明の条件としては、1(1/s))が一定となるように、法線応力検出部および回転速度制御部15において回転速度は自動的にコントロールされる。このようにして減圧下における塗工液の粘度を連続的に測定し、図2に示されるような粘度カーブを得ることができる。図2の粘度カーブにおいて、初期には緩やかに粘度は上昇し、ある時間において急激に粘度変化が起こり、粘度上昇が完了する点21が現れる。この点21は、塗工液の流動性が急速に失われ、塗工液が不動化状態まで変化していることを示し、粘度上昇が完了した時間T1を、測定した塗工液の不動化時間とした。塗工液の不動化時間が長いほど該塗工液の保水度が良好であることを表す。また、Anton Paar社製レオメーターPhysica MCR101のかわりに、同社製MCR301、もしくはMCR501を用いても、同様の結果を得ることができる。
W=(L×r2)/10000 式(1)
式(1)において、L:ラテックスエマルジョンの加圧脱水量(g/m2)、r:ラテックス平均粒子径(nm)である。
(紙基材の調製)
LBKP(フリーネス(CSF)=400ml)70部、NBKP(フリーネス(CSF)=410ml)30部のパルプスラリーに、軽質炭酸カルシウム(PC:白石カルシウム製)を灰分が7部となるように添加し、対パルプ100部当り澱粉1.5部、アルケニル無水コハク酸0.2部、および硫酸バンド0.5部を添加した紙料を用いて長網抄紙機で抄紙し、その抄紙工程中で澱粉の塗工量が乾燥重量で2g/m2となるようにサイズプレス装置で塗布・乾燥させ、マシンキャレンダで旭精工株式会社製全自動デジタル型王研式透気度・平滑度試験機EYOで測定される王研式平滑度を35秒になるように平滑化処理して、坪量が90g/m2の紙基材を得た。この紙基材のPPS平滑は、5.8μmであった。
ミラグロス91(成分;カオリン、エンゲルハード社製)70部に、水および分散剤(商品名;アロンA−9、東亞合成化学社製)0.1部を加え、コーレス分散機にて分散し、固形分72%のカオリン分散液を得た。この分散液に固形分75%のFMT−97(成分;重質炭酸カルシウム、株式会社ファイマテック製)を固形分として30部を加え、顔料スラリーを調製した。この顔料スラリー固形分100部に対して、澱粉(商品名;エースB、澱粉濃度20%・温度40℃におけるB型粘度160mPa・s、王子コーンスターチ社製)1.5部、ラテックス(商品名;T2535D、JSR社製、W値:94、加圧脱水量:70.8g/m2、平均粒子径:115nm、AC3.75部、電解質NaOH/KOH)12部を添加し、さらに水を加えて、固形分濃度が64%の塗工液を調製した。
上記により得られた紙基材に、塗工速度1200m/minである、ジェットファウンテン供給方式のベベルブレードコーターにて、乾燥後の塗工量が片面10g/m2となるように両面に塗工層を設け、坪量110g/m2の塗工紙を得た。
(下塗り塗工液の調製)
ハイドロカーブ60(成分;重質炭酸カルシウム、備北粉化工業株式会社製)100部に、澱粉(商品名;エースB、王子コーンスターチ社製)10部、ラテックス(商品名;XQ83302、ダウ・ケミカル日本株式会社製)4部を添加・撹拌し、さらに水を加えて、固形分濃度が65%の塗工液を調製した。
ミラグロス91(成分;カオリン、エンゲルハード社製)70部に、水および分散剤(商品名;アロンA−9、東亞合成社製)0.1部を加え、コーレス分散機にて分散し、固形分72%のカオリン分散液を得た。この分散液に固形分75%のFMT−97(成分;重質炭酸カルシウム、株式会社ファイマテック製)を固形分として30部を加え、顔料スラリーを調製した。この顔料スラリー固形分100部に対して、澱粉(商品名;エースB、前出)3部、ラテックス(商品名;T2535D、前出)12部を添加し、さらに水を加えて、固形分濃度が64%の塗工液を調製した。
参考例1で得られた紙基材上に、塗工速度1200m/minである、ジェットファウンテン供給方式のベベルブレードコーターにて、乾燥後の塗工量が片面10g/m2となるように下塗り塗工液を両面塗工、乾燥して下塗り層を形成した。この状態での塗工原紙としてのPPS平滑は、4.2μmであった。さらに塗工速度1200m/minである、ジェットファウンテン供給方式のベベルブレードコーターにて、乾燥後の塗工量が片面9g/m2となるように上塗り塗工液を両面塗工、乾燥して塗工層を設け、坪量128g/m2の塗工紙を得た。
参考例2において、上塗り塗工液中のラテックスを異なるラテックス(商品名:PA2327、日本エイアンドエル社製、W値55、加圧脱水量:49.5g/m2、平均粒子径:105nm、AC4.0部)に変更した以外は、参考例2と同様にして塗工紙を得た。
参考例3において、下塗り塗工液中のハイドロカーブ60をハイドロカーブ90(成分;重質炭酸カルシウム、備北粉化工業社製)に変更した以外は、参考例3と同様にして塗工紙を得た。なお、下塗り塗工層形成後の塗工原紙のPPS平滑は、3.5μmであった。
参考例4において、上塗り塗工液濃度を64%から61%に変更した以外は、参考例4と同様にして塗工紙を得た。
参考例4において、上塗り塗工液中のラテックスを異なるラテックス(商品名:S2500B、JSR社製、W値35、加圧脱水量:54.8g/m2、平均粒子径:80nm、AC4.0部、電解質NaOH/KOH)に変更した以外は、参考例4と同様にして塗工紙を得た。
実施例1において、上塗り塗工液中の澱粉配合量を3部から4.5部に変更した以外は、参考例4と同様にして塗工紙を得た。
実施例1において、上塗り塗工液中の澱粉配合量を3部から1.5部に変更した以外は、実施例1と同様にして塗工紙を得た。
実施例1において、上塗り塗工液中の澱粉量を3部から0部とし、さらにアクリル系アルカリ膨潤型合成保水剤(商品名:アルコガムL−29K、日本NSC社製)0.5部を加えた以外は、実施例1と同様にして塗工紙を得た。
実施例1において、下塗り塗工液中のハイドロカーブ90(100部)を、ハイドロカーブ90を50部およびミラグロス91(前出)50部に変更し、固形分濃度を63%に変更し、上塗り塗工液の調製法を下記に変更した以外は、実施例1と同様にして塗工紙を得た。なお、下塗り塗工層形成後の塗工原紙のPPS平滑は、3.1μmであった。
ミラグロス91(成分;カオリン、エンゲルハード社製)50部に、水および分散剤(商品名;アロンA−9、東亞合成社製)0.1部を加え、コーレス分散機にて分散し、固形分72%のカオリン分散液を得た。この分散液に固形分75%のセタカーブHG(成分;重質炭酸カルシウム、備北粉化工業株式会社製)を固形分として50部を加え、顔料スラリーを調製した。この顔料スラリー固形分100部に対して、澱粉(商品名;エースB、前出)2.5部、ラテックス(商品名;S2500B、前出)12部を添加し、さらに水を加えて、固形分濃度が64%の上塗り塗工液を調製した。
実施例4において、上塗り塗工液中のラテックスを異なるラテックス(S2543(B)−2、JSR社製、W値32、加圧脱水量:50.1g/m2、平均粒子径:80nm、AC2.5部、電解質NaOH/KOH)に変更した以外は、実施例4と同様にして塗工紙を得た。
実施例4において、上塗り塗工液中のラテックスを異なるラテックス(S2543(C)−7、JSR社製、W値31、加圧脱水量:48.1g/m2、平均粒子径:80nm、AC2.5部、電解質NaOH)に変更した以外は、実施例4と同様にして塗工紙を得た。
実施例4において、上塗り塗工液中のラテックスを異なるラテックス(S2543(D)−7、JSR社製、W値28、加圧脱水量:43.4g/m2、平均粒子径:80nm、AC2.75部、電解質NaOH、S2543(C)−7に対してAC量を変更し、ポリアクリルアミド存在下で重合)に変更し、さらに澱粉配合量を2.5部から2部に変更した以外は、実施例4と同様にして塗工紙を得た。
参考例2において、上塗り塗工液中の澱粉量を3部から0部とし、ラテックスを14部とした以外は、参考例2と同様にして塗工紙を得た。
参考例2において、上塗り塗工液中のカオリンを異なるカオリン(商品名:コンツァー1500、株式会社イメリスミネラルズジャパン製)に変更してカオリン分散液濃度を63%とし、上塗り塗工液濃度を61%とした以外は、参考例2と同様にして塗工紙を得た。
塗工液のハイシェア粘度は、熊谷理機工業株式会社製ハーキュレス高せん断粘度型Model HR−801Cを用い、ボブF、回転数8800回転での粘度を測定した。この際のせん断速度は、1.8×105(1/s)である。
Anton Paar社製レオメーターPhysica MCR101と同社のイモビリゼーションセルとを組み合わせてなる塗工液の不動化時間を測定する装置を使用して測定した。測定条件は、測定治具としてパラレルプレート50mmφ、初期ギャップ0.5mm、測定中せん断速度1(1/s)一定とし、減圧度700hPaとして、減圧開始後に塗工液粘度の測定を行い、塗工液粘度が急激に上昇し、上昇を完了した時間を測定した塗工液の不動化時間とした。塗工液容量は2mlとし、紙基材としては本発明で規定した、特定の紙基材を使用した。
ラテックスの加圧脱水量は、Kaltec Scientific,Inc.製のAA−GWR保水度計を用いて測定した。測定条件としては、印加圧力100kPa、加圧時間30秒にて加圧し、0.1μmポアサイズポリカーボネートフィルターを介して濾紙No.2にラテックス中水分を吸収させ、測定前後のろ紙重量変化から、ラテックスの加圧脱水量(g/m2)を求めた。なお、加圧脱水量は固形分濃度により大きく変動するため、ラテックスの加圧脱水量測定においては、該エマルジョンの固形分濃度を50%に統一し、測定するラテックスの温度を25℃として測定した。
ラテックスをオスミウム酸で処理し、これを透過型電子顕微鏡で倍率5万倍で写真撮影し、得られた顕微鏡写真の重合体ラテックス粒子の約200個の粒子径を測定し数平均で求めた。
TAPPI試験法:T 480 om−92(TAPPI Test Method T 480 om−92)に準じて、光沢度計(型式:GM−26D、村上色彩技術研究所社製)を使用して測定した。
各実施例・比較例で使用した塗工用原紙、および得られた塗工紙の平滑度を、パーカープリントサーフ(PPS)表面平滑度試験機(機種:MODEL M−569型、MESSMER BUCHEL社製/英国)を用い、バッキングディスク:ソフトラバー、クランプ圧力:1MPaで5回平滑度測定を行ない、その平均を求めた。
塗工紙のストリーク発生状況に対して、下記のように評価を行った。
◎:ストリークの発生がなく、全く問題ないレベルである。
○:ストリークがわずかに発生したが、実用上問題とならないレベルである。
×:ストリークが頻繁に発生し、生産効率に劣り、問題となるレベルである。
11b レオメーターパラレルプレート下部
13a 減圧室
13b 減圧ポンプ接続口
15 レオメーター法線応力検出部および回転速度制御部
17 測定対象塗工液
19 紙基材
21 塗工液不動化完了点
Claims (7)
- セルロース繊維を主体とする紙基材の少なくとも一面上に、顔料および接着剤を主成分とする塗工液を塗工、乾燥して得られる塗工層を少なくとも1層以上設けてなる顔料塗工紙の製造方法において、前記紙基材がPPS平滑4.0μm以下の平滑度を有し、前記塗工液に、顔料として炭酸カルシウムが顔料全固形分に対して5〜100質量%含有し、かつ接着剤として、平均粒子径が50〜100nmであり、Kaltec Scientific,Inc.製のAA−GWR保水度計を用いて下記の条件(1)で測定される加圧脱水量L値が15〜70g/m 2 であり、かつ下記(2)で計算されるW値が10〜70であるラテックスを顔料全固形分に対して5〜25質量%含有して、さらに該塗工液が、せん断速度1.8×105(1/s)で測定されるハイシェア粘度が40mPa・s以下であり、Anton Paar社製レオメーターPhysica MCR101と同社のイモビリゼーションセルとを組み合わせてなる装置を使用して下記の条件(3)で測定される塗工液の不動化時間が200〜4000秒であることを特徴とする顔料塗工紙の製造方法。
(1)測定条件:印加圧力:100kPa、加圧時間:30秒、フィルター:0.1μmポアサイズ
(2)W値=(L×r2)/10000
L:加圧脱水量(g/m2)、r:ラテックス平均粒子径(nm)
(3)測定条件:減圧度:700hPa、せん断速度:1(1/s)、初期ギャップ:0.5mm - 前記ラテックスの重合に使用されるエチレン系不飽和カルボン酸単量体量が、全モノマー100質量部中3.5質量部以下である、請求項1に記載の顔料塗工紙の製造方法。
- 前記ラテックスの配合量が、顔料全固形分に対して5〜25質量%である、請求項1または2に記載の顔料塗工紙の製造方法。
- 前記接着剤において、更に澱粉が含有され、澱粉含有量が顔料全固形分に対して0.5〜3質量%以下である、請求項1〜3のいずれか1項に記載の顔料塗工紙の製造方法。
- 前記澱粉が、濃度20%、温度40℃にて測定された粘度が30mPa・s以上である、請求項4に記載の顔料塗工紙の製造方法。
- 前記紙基材上に塗工層を設ける方法がブレード塗工方式である、請求項1から5のいずれか1項に記載の顔料塗工紙の製造方法。
- 前記紙基材が、あらかじめ顔料および接着剤を主成分とする下塗り塗工層を少なくとも1層以上設けたものである、請求項1から6のいずれか1項に記載の顔料塗工紙の製造方法。
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