JP2009108466A - 紙の表面処理剤 - Google Patents
紙の表面処理剤 Download PDFInfo
- Publication number
- JP2009108466A JP2009108466A JP2008265143A JP2008265143A JP2009108466A JP 2009108466 A JP2009108466 A JP 2009108466A JP 2008265143 A JP2008265143 A JP 2008265143A JP 2008265143 A JP2008265143 A JP 2008265143A JP 2009108466 A JP2009108466 A JP 2009108466A
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Abstract
【解決手段】紙の表面処理剤は、特定のビニル単量体と特定のカチオン性基含有ビニル単量体とを特定のモル比で重合することにより得られる、あるいは、特定のビニル単量体と特定のカチオン性基含有ビニル単量体と架橋性ビニル単量体を特定のモル比で重合することにより得られる、カチオン性基含有共重合体である。該カチオン性基含有共重合体を塗工した原紙に、顔料と接着性を主成分とする塗工液を塗工し、塗工紙。
【選択図】なし
Description
本発明に係るカチオン性基含有共重合体は、(A):上記一般式(I)及び(II)で表されるビニル単量体から選ばれる少なくとも1種と、(B):上記一般式(III)及び(IV)で表されるカチオン性基含有ビニル単量体から選ばれる少なくとも1種とを、所定のモル比で重合することにより得られる。
本発明に係るカチオン性基含有共重合体は、一般式(I)及び(II)で表されるビニル単量体から選ばれる少なくとも1種を構成成分とする。
本発明に係るカチオン性基含有共重合体は、一般式(III)及び(IV)で表されるカチオン性基含有ビニル単量体から選ばれる少なくとも1種を構成成分とする。
本発明に係るカチオン性基含有共重合体は、(A)成分と(B)成分の組成比率(モル比)が(A)成分/(B)成分で、97/3〜30/70であり、好ましくは、97/3〜40/60である。これらの組成比率内にある場合は、顔料と接着剤を主成分とする塗工液を塗工した際、塗工液の一部が凝集すること、また共重合体が瞬時に塗工液中の水分を吸収することから、塗工液の紙内部への浸透を抑制し得るといった効果が発現される。さらに、上記組成比率内にある場合には、表面処理剤の紙表面への接着力が向上し、原紙と塗工層の剥離強度低下を十分に抑制し得る。
本発明に係るカチオン性基含有共重合体は、必要に応じて、(C)成分として、架橋性ビニル単量体〔但し、前記一般式(IV)で表される単量体を除く〕も構成成分とすることができる。架橋性ビニル単量体は、好ましくは、ビニル基、アクリロイル基、メタクリロイル基及びアリル基から選ばれる少なくとも2個の基を分子中に有する。少なくとも2個のビニル基を分子中に有する架橋性ビニル単量体としては、エチレングリコールジ(メタ)アクリレート、ジエチレングリコールジ(メタ)アクリレート、ポリエチレングリコールジ(メタ)アクリレート、プロピレングリコールジ(メタ)アクリレート、ジプロピレングリコールジ(メタ)アクリレート、ポリプロピレングリコールジ(メタ)アクリレート、1,2 −ブチレングリコールジ(メタ)アクリレート、1,3 −ブチレングリコールジ(メタ)アクリレート、ネオペンチルグリコールジ(メタ)アクリレート、グリセリンジ(メタ)アクリレート、グリセリントリ(メタ)アクリレート、トリメチロールプロパントリ(メタ)アクリレート、ペンタエリスリトールテトラ(メタ)アクリレート等の多価アルコールの(メタ)アクリル酸エステル類;N−メチルアリルアクリルアミド、N−ビニルアクリルアミド、N,N’−メチレンビス(メタ)アクリルアミド、ビスアクリルアミド酢酸等のアクリルアミド類;ジビニルベンゼン、ジビニルエーテル、ジビニルエチレン尿素等のジビニル化合物;ジアリルフタレート、ジアリルマレート、ジアリルアミン、トリアリルアミン、トリアリルアンモニウム塩、ペンタエリスリトールのアリルエーテル化体、分子中に少なくとも2個のアリルエーテル単位を有するスクローゼのアリルエーテル化体等のポリアリル化合物;ビニル(メタ)アクリレート、アリル(メタ)アクリレート、2−ヒドロキシ−3−アクリロイルオキシプロピル(メタ)アクリレート等の不飽和アルコールの(メタ)アクリル酸エステルなどが挙げられる。
本発明に係るカチオン性基含有共重合体は、前記の少なくとも2種類のビニル単量体を必須構成成分とし、好ましくは更に前記架橋性ビニル単量体を構成成分とする共重合体であるが、これらビニル単量体と共重合可能な他のビニル単量体も構成成分とすることができる。
本発明に係るカチオン性基含有共重合体を製造する方法については必ずしも制限はないが、通常は水溶液重合法、逆相懸濁重合法、沈澱重合法などの方法によることが好ましい。例えば、水溶液重合法としては、水又は水と均一に混合可能な親水性有機溶媒或いはこれらの混合溶媒等の溶媒中に単量体成分、架橋剤を均一に溶解し、窒素、炭酸ガス等の不活性ガスによる置換等により系内の溶存酸素を除去した後、重合開始剤を添加して反応させる方法が挙げられる。重合開始温度は通常20〜90℃程度であり、反応時間は1〜10時間程度である。単量体として水に溶け難い成分を使用する場合、親水性有機溶媒を併用するのが望ましい。
表1の単量体を用いてカチオン性基含有共重合体を以下の方法で製造した。
1Lビーカーにイオン交換水267.4g、MOEDES(ジメチルアミノエチルメタクリレートとジメチル硫酸の当モル付加物(有効分80重量%)。いずれも試薬、和光純薬工業(株)製)185.63g(有効分148.50g)、DMAAm(N,N−ジメチルアクリルアミド、試薬、和光純薬工業(株)製)110.46g、NK−14G(架橋剤、ポリエチレングリコールジメタクリレート、新中村化学(株)製)0.415g、V−50(重合開始剤、2,2'−アゾビス(2−アミジノプロパン)・2塩酸塩、和光純薬工業(株)製)0.952gを混合し、モノマー水溶液Aとした。5Lのガラス容器にシクロヘキサン1648g、分散剤としてシュガーエステルS−770(三菱化成(株)製)を1.94g仕込み、60℃で1時間かけ均一に溶解せしめた。溶解後、30℃に冷却し、分散剤溶液Bとした。
カチオン性基含有共重合体の製造例1に順じ、表1に示すモノマー組成でカチオン性基含有共重合体2(平均粒子径3.8μm)、および3(平均粒子径5.1μm)を製造した。
内容積1リットルで、ジャケットに70℃のオイルを外部循環させたシグマ型攪拌腕を2本有するステンレス製ニーダー中に、DADMAC(ジアリルジメチルアンモニウムクロライド、65%水溶液、ダイソー(株)製)45.92g(固形分29.85g)、アクリルアミド(AAm、試薬、和光純薬工業(株)製)48.28g、NK−14G(架橋剤、ポリエチレングリコールジメタクリレート、新中村化学(株)製)0.0214g、イオン交換水350gからなるあらかじめ窒素置換したモノマー水溶液を入れ、20〜40分さらに窒素ガスを吹き込み反応系内を窒素置換しながら、モノマー水溶液の昇温を行った。ついで、重合開始剤としてV−50を0.22g添加した。重合開始剤を添加してから15分後から増粘し、1時間後に系全体が柔らかいゲル状となった。そのまま4時間重合を継続させた。餅状の重合物を取り出し、95℃で乾燥させた。その後、コーヒーミル、ジェットミルで粉砕した。粉砕した架橋粒子をハイボルターで分級し、カチオン性基含有共重合体4を得た。(平均粒子径45μm)
1Lの攪拌機と温度計、冷却管の付いたガラス容器にイオン交換水155.38gを仕込み、窒素置換後、昇温し、70℃とした。別の500mLビーカーに、78%QDM(ジメチルアミノエチルメタクリレートのメチルクロライド四級化物、三菱レイヨン(株)製)53.33gとAAm(アクリルアミド、試薬、和光純薬工業(株)製)56.81g、MBAAm(メチレンビスアクリルアミド、試薬、和光純薬工業(株)製)0.1541g、およびイオン交換水49.38gを混合溶解せしめ、1時間にわたり滴下した。並行しV−50 1.38gをイオン交換水59.57gに溶解し、モノマーと別口から1時間で滴下した。さらに70℃で6時間熟成した後、室温に冷却した。有効分濃度24.4%、カチオン性基含有共重合体5の水溶液を得た。
製造例5に準じ、AAm56.81gを56.88gに、架橋剤MBAAm(メチレンビスアクリルアミド)を添加せず、他の条件は変更せずに製造した。有効分濃度24.2%、カチオン性基含有共重合体6の水溶液を得た。
カチオン性基含有共重合体の製造例1に順じ、表1に示すモノマー組成でカチオン性基含有共重合体7(平均粒子径3.8μm)、および8(平均粒子径4.3μm)を製造した。
カチオン性基含有共重合体の製造例1に順じ、表1に示すモノマー組成で比較のカチオン性基含有共重合体9(平均粒子径5.2μm)、10(平均粒子径5.2μm)、11(平均粒子径5.5μm)、および12(平均粒子径4.5μm)を製造した。
5Lの攪拌機と温度計、冷却管の付いたガラス容器に85%イソプロピルアルコール995g仕込み、攪拌をしつつ20%水酸化ナトリウム44.4g、イオン交換水243g、コーンスターチ(三和澱粉工業(株)製)1000gを加え、室温で分散させた。グリシジルトリメチルアンモニウムクロリド水溶液〔あらかじめHAC−65(東邦化学工業(株)製)150gに20%水酸化ナトリウム95.7gを滴下・混合10分間したもの〕245.7gを滴下後、窒素置換し、次いで昇温し、50℃とした。10時間カチオン化反応した後、35%塩酸21.3gを加え中和した。さらに35%塩酸23.2gを加え、40℃で10時間切断反応を行った。次いで3%水酸化ナトリウム276gでpH6に調整し、冷却後、ヌッチェで濾過した。濾過残にイソプロピルアルコール1000g加え、室温で攪拌抽出と濾過を5回繰り返した後、50℃で減圧乾燥し、カチオン化澱粉1000gを得た。N%(ケルダール法)は0.60%であり、5%水溶液粘度(at.50℃)は50mPa・sであった。
(1)原紙1(表中、手抄き紙と表記)
<パルプ原料>
パルプ原料としては、LBKP(広葉樹晒パルプ)を、25℃で叩解機にて離解、叩解して2.2重量%のLBKPスラリーとしたヴァージンパルプを用いた。このもののカナダ標準濾水度(JIS P 8121)は450mlであった。
ヴァージンパルプスラリーを抄紙後のパルプシートのパルプ坪量が80g/m2±1g/m2になるように量り取り、角型タッピ抄紙機にて80メッシュワイヤー(面積625cm2)で抄紙し、パルプシートを得た。抄紙後のシートは、3.5kg/cm2で5分間プレス機にてプレスし、鏡面ドライヤーを用い105℃で2分間乾燥した。乾燥されたパルプシートを23℃、湿度50%の条件で1日間調湿し、表面処理に供する原紙とした。原紙嵩密度は0.574g/cm3であった。
実機紙(坪量が43g/m2±1g/m2)を表面処理に供する原紙とした。原紙嵩密度は0.750g/cm3であった。
ヴァージンパルプスラリーに内添剤を添加した以外は原紙1と同様にして得た手抄き紙(パルプ坪量が80g/m2±1g/m2)を、表面処理に供する原紙とした。原紙嵩密度は0.574g/cm3であった。
(1)方法1
ガラス板上にワイヤーコーターで、表面処理剤として表中に示す成分を所定濃度で含有する水溶液を用い、50g/m2のキャスティング皮膜を形成した。次いで上記原紙(幅12.5cm×長さ25cm)をキャスティング皮膜上にのせ、100g/m2のろ紙一枚でカバーし、ロール(直径200mm、幅200mm、線圧230g/cm)を転がし、表面処理剤をガラス板上から原紙表面に転写(塗布)した。次いで鏡面ドライヤーを用い105℃で2分間乾燥した。これらの一連の操作は間髪をいれずすみやかに操作した。乾燥されたパルプシートを23℃、湿度50%の条件で1日間調湿し、塗工原紙とした。なお、水溶液濃度等は塗布量(固形分換算)が表中の数値となるように調整した。
ゲートロールコーター(PM−9002GC、処理速度300m/分、(株)エスエムテー製)を用い、表面処理剤として表中に示す成分を所定濃度で含有する水溶液を、上記原紙(実機原紙)に表面処理(塗布)を施し、105℃、20秒間鏡面ドライヤーを用い乾燥した。乾燥されたパルプシートを23℃、湿度50%の条件で1日間調湿し、塗工原紙とした。なお、水溶液濃度等は塗布量(固形分換算)が表中の数値となるように調整した。
エースA:酸化澱粉、王子コンスターチ(株)製
cato308:カチオン化澱粉、紙力増強・紙質改善剤、日本エヌエスシー(株)製
GL−05:部分ケン化ポリビニルアルコール、日本合成(株)製
WS−4020:ポリアミドエピクロルヒドリン樹脂、有効分25%、星光PMC(株)製
塗料(1%):下記で用いた塗工紙用塗工液(有効分濃度65%)を水で有効分濃度1%に希釈したもの
ポリマロン482S:オレフィン系樹脂、表面サイズ剤、有効分25%、荒川化学(株)製
上記で得られた塗工原紙(表面処理紙)の片面に、塗工液を、ブレード式の塗工機(フレキシブルトレーリングブレードコーター、塗工速度140m/分、塗工圧0.5〜1.5kg/cm2、熊谷理機工業(株)製)にて塗工し、105℃、20秒間鏡面ドライヤーを用い乾燥した。
<表面処理剤の塗布量>
表面処理剤の処理で得られた塗工原紙(表面処理紙)と、表面処理前の原紙を、それぞれ23℃、湿度50%の条件で1日間調湿し、その差分をサンプルの面積(幅12.5cm×長さ25cm)で除した値から塗布量(g/m2)を算出した(測定枚数3の平均値)。表面処理剤による塗布を行わないものは、塗布量を0g/m2とした。
塗工紙の製造で得られた塗工紙を幅12.0cm×長さ24cmにカットしたサンプルと、表面処理剤の処理で得られた塗工原紙(表面処理紙)(幅12.5cm×長さ25cm)を、それぞれ23℃、湿度50%の条件で1日間調湿し、それぞれ坪量を算出した後、(塗工紙の坪量−表面処理紙の坪量)の値から塗工量(g/m2)を算出した(測定枚数3の平均値)。
JIS P8142に従って光沢度計(GMX−203型、75°型、(株)村上色彩技術研究所製)を用い、塗工面の白紙光沢度を測定し、その平均値を求めた(測定ヶ所数6/1枚、測定枚数3枚、18点の平均値)。光沢度が大きいほど、光沢性が高く、また光沢度の1%(1ポイント)の差は有意差として十分に認識されるものであり、差が3%(3ポイント)になると相違は更に顕著となる。
JIS P8118により、緊度を測定し、嵩密度とした(測定枚数3の平均値)。嵩密度が小さいほど、軽量であり、また嵩密度の0.02の差は有意差として十分に認識されるものである。
JIS P8139に従ってインターナルボンドテスター(熊谷理機工業(株)製)により、剥離強度を測定し、Z軸剥離強度とした(測定ヶ所数5/1枚、測定枚数2の平均値)。数値が大きいほど剥離強度が高い。
・カチオン化澱粉:紙力増強・紙質改善剤、商品名「cato308」、日本エヌエスシー(株)製
・硫酸バンド:硫酸アルミニウム水溶液、キシダ化学(株)製
・アルキルケテンダイマー:サイズ剤、商品名「AD1603」、星光PMC(株)製
Claims (6)
- (A):一般式(I)で表されるビニル単量体及び一般式(II)で表されるビニル単量体から選ばれる少なくとも1種〔以下、(A)成分という〕と、(B):一般式(III)で表されるカチオン性基含有ビニル単量体及び一般式(IV)で表されるカチオン性基含有ビニル単量体から選ばれる少なくとも1種〔以下、(B)成分という〕とを、(A)成分/(B)成分で97/3〜30/70のモル比で重合することにより得られるカチオン性基含有共重合体を含有する、紙の表面処理剤。
〔式中、R1は水素原子又はメチル基を示し、R2及びR3は同一又は異なって、水素原子又は炭素数1〜4の直鎖状もしくは分岐状のアルキル基又はアルケニル基を示す。〕
〔式中、R1は前記の意味を示し、A1及びA2は同一又は異なって、式-(CH2)n-(nは2〜6の整数を示す)で表される基を示し、Bは-O-又は-CH2-基を示す。〕
〔R1は前記の意味を示し、R4及びR5は同一又は異なって、炭素数1〜4のアルキル基又はアルケニル基を示し、R6は水素原子又は炭素数1〜4のアルキル基を示し、Yは-O-、-NH-又は-O-CH2CH(OH)-基を示し、Zは炭素数1〜4の直鎖状又は分岐状のアルキレン基を示し、Xは酸の共役塩基、ハロゲン原子又は炭素数1〜4のアルキルサルフェート基を示す。〕
〔式中、R7及びR8は同一又は異なって水素原子又はメチル基を示し、R9及びR10は同一又は異なって水素原子又は炭素数1〜4のアルキル基を示し、Xは前記の意味を示す。〕 - 前記カチオン性基含有共重合体が、(A)成分と、(B)成分と、更に(C):架橋性ビニル単量体〔但し、前記一般式(IV)で表される単量体を除く〕〔以下、(C)成分という〕とを重合することにより得られる、請求項1に記載の紙の表面処理剤。
- (A)成分が、(メタ)アクリルアミド、N,N−ジメチル(メタ)アクリルアミド及びN,N−ジエチル(メタ)アクリルアミドから選ばれる少なくとも1種以上である請求項1又は2記載の紙の表面処理剤。
- 前記カチオン性基含有共重合体における(C)成分の量が、(A)成分、(B)成分及び(C)成分の合計中、0.0005〜5モル%である請求項2又は3記載の紙の表面処理剤。
- 請求項1〜4記載の紙の表面処理剤を、パルプを主原料とする紙の少なくとも片面に、片面当たり、乾燥重量で0.01〜3.0g/m2処理した塗工原紙。
- 請求項5記載の塗工原紙の前記表面処理剤による処理面に、顔料と接着剤を主成分とする塗工液の塗工層を設けてなる、密度が1.5g/cm3以下である塗工紙。
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EP (1) | EP2199463A4 (ja) |
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Cited By (2)
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JP2010196217A (ja) * | 2009-02-27 | 2010-09-09 | Nippon Paper Industries Co Ltd | グラビア印刷用塗工紙 |
KR101946221B1 (ko) * | 2010-11-05 | 2019-02-08 | 솔레니스 테크놀러지스 케이맨, 엘.피. | 종이 강도 개선을 위한 중합체의 표면 적용 |
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US9475329B2 (en) * | 2011-07-29 | 2016-10-25 | Hewlett-Packard Development Company, L.P. | Print medium surface treatment |
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EP3553147B1 (en) * | 2016-12-14 | 2022-05-11 | Tokyo Ohka Kogyo Co., Ltd. | Surface treatment liquid and surface treatment method |
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CN101821453B (zh) | 2012-07-04 |
JP5261126B2 (ja) | 2013-08-14 |
WO2009048179A1 (ja) | 2009-04-16 |
US20100273016A1 (en) | 2010-10-28 |
EP2199463A1 (en) | 2010-06-23 |
CN101821453A (zh) | 2010-09-01 |
EP2199463A4 (en) | 2012-10-17 |
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